CN102295285A - Recovery method of silicon slice cutting waste mortar - Google Patents
Recovery method of silicon slice cutting waste mortar Download PDFInfo
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- CN102295285A CN102295285A CN2010102145346A CN201010214534A CN102295285A CN 102295285 A CN102295285 A CN 102295285A CN 2010102145346 A CN2010102145346 A CN 2010102145346A CN 201010214534 A CN201010214534 A CN 201010214534A CN 102295285 A CN102295285 A CN 102295285A
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Abstract
The invention provides a recovery method of silicon slice cutting waste mortar. The method comprises the following steps: a, carrying out solid-liquid separation on the silicon slice cutting waste mortar to obtain a solid sand material and a liquid; b, adding a decoloring agent, an ion adsorbent and a filter aid in the liquid obtained in the step a, and carrying out solid-liquid separation so as to obtain a polyethylene glycol cutting recovery liquid; c, removing metals in the solid sand material obtained in the step a through magnetic separation so as to obtain a mixture of silicon and silicon carbide; and d, carrying out vacuum heating on the mixture of silicon and silicon carbide obtained in the step c at the temperature of 1425-1550 DEG C, cooling to room temperature, filtering with a sieve, collecting substances under the sieve so as to obtain silicon carbide micropowder, collecting substances on the sieve so as to obtain silicon blocks, and smashing the silicon blocks so as to obtain silicon powder. The recovery method provided by the invention is extremely environmentally-friendly and can be used for thoroughly separating out silicon and silicon carbide, and the purities of recovered polyethylene glycol, silicon carbide and silicon powder are high.
Description
Technical field
The present invention relates to a kind of recovery method of silicon chip dicing waste mortar.
Background technology
In the cutting process of single crystalline Si, polycrystalline Si, the metal powder that produces after the silica flour that produces during the cutting silicon rod, broken silicon-carbide particle, the steel wire grinding deposits in the mortar, forms waste mortar, and its cutting ability reduces greatly.Waste mortar is recycled, extract wherein silica flour, silicon carbide micro-powder and polyoxyethylene glycol, recycling, the purpose that can play save energy, cuts the waste.The method that waste mortar is reclaimed mainly contains (1) centrifuging at present: centrifugation, remove invalid silicon carbide abrasive and silica flour broken in the waste mortar; (2) chemical method: pharmaceutical chemicalss such as employing acid/alkali are removed silica flour and the metallic impurity in the waste mortar.
But the separation efficiency of centrifuging is lower, and chemical method adopts a large amount of acid/alkali, and the cost height has very big harm to environment; In addition, centrifuging, chemical method all can only reclaim polyoxyethylene glycol and the silicon carbide micro-powder in the mortar, to the effective recycling of the energy of the high purity silicon powder in the waste mortar, have caused great waste.Begin to seek to reclaim the whole bag of tricks of silicon, carborundum powder and polyoxyethylene glycol in the prior art.
CN101691224A discloses a kind of silicon chip cutting mortar recovery method, and (1) obtains efflux of solids and liquid flow by the physics cyclonic separation; (2) liquid flow adopts by decolouring, ionic adsorption, filters, and can obtain polyoxyethylene glycol; (3) efflux of solids obtains lighter silicon stream and heavier silicon carbide stream by gravity settling separation; (4) silicon stream washs, is drying to obtain silica flour; The macrobead that screens out in the silicon carbide stream obtains silicon carbide.But have the less silicon-carbide particle of particle diameter in the waste mortar, close with the silicon grain quality, the silica flour that causes gravity separation to reclaim obtaining and the purity of silicon carbide micro-powder are lower; Especially be adsorbed on lip-deep fine silica powder particle of silicon-carbide particle and the silicon-carbide particle that is adsorbed, often be difficult to separate fully.
CN101130237A discloses a kind of method that reclaims silica flour and carborundum powder from waste mortar, and (1) solid-liquid separation obtains the mortar throw out, adds suspension agent and binding agent molecule in the acetone solution throw out, and centrifugation obtains the sand powder; (2) air-flow flotation obtains silica flour and silicon carbide/metal mixed powder; (3) add the liquid of density between silicon and silicon carbide and carry out flotation, the flotation thing is a silica flour, and throw out is silicon carbide/metal mixed powder; (4) silica flour washing, drying obtain the HIGH-PURITY SILICON particulate; Silicon carbide/metal mixed powder is isolated metal by magnetic separation, obtains carborundum powder.This method is carried out flotation by selecting the liquid of density between silicon and silicon carbide, but the particle diameter of the silicon carbide that is broken in the waste mortar is very little, the silicon carbide micro-powder that these particle diameters are little in the actual mechanical process can be carried to float to the liquid upper strata together or carried to be dispersed in the process by silica flour and cause last layering not obvious in the middle of the liquid by silica flour, adopts the silicon-carbide particle that also contains 10-13wt% in the silica flour after this method is separated.Therefore, the isolating purity of liquid floatation is still lower.Simultaneously, the various liquid costs that adopt during liquid floatation are very high, and toxicity is very big, and there is harm in human and environment.
Summary of the invention
The invention solves the silicon that exists in the prior art and separate not thoroughly with silicon carbide, and there is the technical problem of harm in separating technology to human and environment.
The invention provides a kind of recovery method of silicon chip dicing waste mortar, may further comprise the steps:
A. the silicon chip dicing waste mortar solid-liquid separation obtains solid sand material and liquid part;
B. add discoloring agent, ion adsorbent and flocculating aids in the liquid part that obtains among the step a, solid-liquid separation obtains the polyoxyethylene glycol cutting and reclaims liquid;
C. the solid sand material that obtains among the step a separates by magnetic separation removes metal, obtains the mixture of silicon and silicon carbide;
D. with the mixture of the silicon that obtains among the step c and silicon carbide 1425-1550 ℃ of following heating under vacuum; Be cooled to screen cloth vibration filtering after the room temperature, collect undersized material and obtain silicon carbide micro-powder, the material on the collection screen obtains silico briquette; Pulverize silico briquette and obtain silica flour.
In the recovery method of silicon chip dicing waste mortar provided by the invention, first solid-liquid separation obtains solid sand material and liquid part, and liquid part obtains the higher polyoxyethylene glycol of purity by decolouring, ionic adsorption; Solid part is separated the removal metallic impurity by magnetic separation earlier, by pyroprocessing divided silicon and silicon carbide, need not to use other pharmaceutical chemicalss then, and the technology simple controllable does not have harm to people, environment; The temperature heating separates between silicon and silicon carbide fusing point by selecting, the complete vitreous clinker of silica flour, and silicon carbide still is pulverulence, thus make silicon thoroughly separate with silicon carbide, purity is very high.The present invention reclaims polyoxyethylene glycol and the silicon carbide that obtains, and can directly continue on for the silicon chip cutting; And the purity that reclaims the silica flour that obtains is also higher, can be used as the starting material that silicon single crystal or polysilicon silicon ingot are made.
Embodiment
The invention provides a kind of recovery method of silicon chip dicing waste mortar, may further comprise the steps:
A. the silicon chip dicing waste mortar solid-liquid separation obtains solid sand material and liquid part;
B. add discoloring agent, ion adsorbent and flocculating aids in the liquid part that obtains among the step a, solid-liquid separation obtains the polyoxyethylene glycol cutting and reclaims liquid;
C. the solid sand material that obtains among the step a separates by magnetic separation removes metal, obtains the mixture of silicon and silicon carbide;
D. with the mixture of the silicon that obtains among the step c and silicon carbide 1425-1550 ℃ of following heating under vacuum; Be cooled to screen cloth vibration filtering after the room temperature, collect undersized material and obtain silicon carbide micro-powder, the material on the collection screen obtains silico briquette; Pulverize silico briquette and obtain silica flour.
According to recovery method of the present invention, earlier silicon chip dicing waste mortar is carried out solid-liquid separation.Mainly contain silicon-carbide particle, polyoxyethylene glycol in the former mortar in the waste mortar of silicon chip cutting, the silicon-carbide particle and the metallic impurity of the silica flour that produces in the working angles, fragmentation.Solid-liquid separation can adopt plate-and-frame filter press, Membrane filtering machine or whizzer to finish.Because silicon, silicon carbide particle diameter are less, so the present invention preferably adopts whizzer to carry out solid-liquid separation.More preferably under the situation, during centrifugation, centrifugal rotational speed is 1000-2000rpm, centrifugation time 20-40min.
After the solid-liquid separation, obtain solid sand material and liquid part, wherein mainly contain silica flour, silicon carbide micro-powder and metallic impurity in the solid sand material, be mainly polyoxyethylene glycol in liquid part.Add discoloring agent, ion adsorbent and flocculating aids in liquid part, continue solid-liquid separation, promptly obtain the polyoxyethylene glycol cutting and reclaim liquid, this polyoxyethylene glycol cutting is reclaimed liquid and can be continued to use with silicon chip and cut.
Under the preferable case, the mode that discoloring agent and ion adsorbent can adopt substep to add; For example, in liquid part, add discoloring agent and flocculating aids earlier, adopt filtering centrifuge to carry out solid-liquid separation, remove filter residue, in filtrate, add ion adsorbent and flocculating aids then, behind the reaction 1-10h, adopt filtering centrifuge to carry out solid-liquid separation, remove filter residue and can obtain polyoxyethylene glycol cutting recovery liquid.Similarly, also can add ion adsorbent and flocculating aids, filtering separation earlier; And then adding discoloring agent and flocculating aids, filtering separation obtains polyoxyethylene glycol.
Wherein, discoloring agent is gac and/or ammonium persulphate, and ion adsorbent is polyacrylamide or Poly Dimethyl Diallyl Ammonium Chloride, and flocculating aids is diatomite or perlite.Quality is than liquid part: discoloring agent: ion adsorbent: flocculating aids=(10-5): 1: 1: 1.
Mainly contain silica flour, silicon carbide micro-powder and metallic impurity in the solid sand material.Among the present invention, separate the metallic impurity of removing in the solid sand material by magnetic separation earlier.Described magnetic separation separates can directly adopt various magnetic graders in the prior art.In the magnetic separation separate solid sand material, obtain the mixture of silicon and silicon carbide.
Among the present invention, adopt in the high temperature sorting mixture silicon and silicon carbide.The silica flour fusing point is 1410 ℃; About 2700 ℃ of silicon carbide fusing point is far above the fusing point of silica flour; Therefore when Heating temperature is between silica flour fusing point and silicon carbide fusing point, silica flour in the mixture can fusion be liquid-phase silicone stream, and silicon carbide still is pulverulence mutually, because solid-liquid biphase interfacial tension, the molten silicon stream aggregation that closes on forms tangible separation surface to together with the silicon carbide solid; Then mixture system is cooled to room temperature, the silicon stream caking that is brought together forms the relatively large silico briquette of volume, and can separate silicon and silicon carbide by screen filtration this moment.Be cooled in the room temperature process, the silico briquette surface can attach the small amount of carbonized silicon grain, and the silicon-carbide particle that this can be attached when the screen cloth vibration filtering removes.
For preventing that silica flour high temperature and airborne oxygen or nitrogen from reacting, described heat-processed need be carried out in a vacuum.The heating under vacuum temperature is 1425-1550 ℃ among the present invention.Under the preferable case, the temperature of heating under vacuum is 1450-1480 ℃, and vacuum tightness is not higher than-0.01MPa; The time of heating under vacuum is 3-6h.After heating under vacuum is finished, to be cooledly to room temperature, discharge vacuum again, prevent silico briquette surface oxidation or nitrogenize.
Among the present invention, the mixture of silicon and silicon carbide can be placed crucible, carry out heating under vacuum then.Because the heating under vacuum temperature is higher, so the present invention has relatively high expectations to crucible.Described crucible can adopt quartz crucible or alumina-ceramic crucible, and crucible internal layer surface is covered with silicon nitride layer.Silicon nitride in air, be heated to 1450-1550 ℃ still very stable, therefore can satisfy the requirement of heating under vacuum of the present invention.In addition, silicon nitride layer can also prevent the bonding of mixture and crucible in the high-temperature heating process.
After heating under vacuum is finished, be cooled to room temperature earlier, by the screen cloth vibration filtering, the material on the collection screen obtains the silico briquette of vitreous clinker then, collects undersized material and obtains still being that the silicon carbide micro-powder of powder shaped, this silicon carbide can continue on for the silicon chip cutting.During the screen cloth vibration filtering, because the silicon carbide micro-powder particle grain size that is adopted in the former mortar is all at 100 μ m and following, and the silico briquette size after the fusion reaches more than the millimeter level, so the screen mesh size that the present invention selects for use is the 100-300 order, and the screen cloth vibrational frequency is 40-80 time/min.
Collect the silico briquette that obtains on the sieve, can adopt various breaking method of the prior art to pulverize, thereby the silica flour that obtains reclaiming can be used as the starting material that silicon single crystal or polysilicon silicon ingot are made.Among the present invention, preferably adopt the comminution by gas stream silico briquette, be about to silico briquette and change in the mill chamber of micronizer mill, be crushed to required particle diameter.Stream pressure in the mill chamber is 0.5-0.7MPa; The time 5-20min of comminution by gas stream.
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Prepare waste mortar by following composition: cutting liquid 44wt%, silicon carbide micro-powder 48wt%, silica flour 6.8wt%, metallic particles 1.2wt%.
(1) with the rotating speed centrifugation 40min of 10Kg waste mortar, obtains liquid and solid sand material with 1400rpm.In liquid, add 440g polyacrylamide and 440g diatomite, the rotating speed centrifuging of back with 1400rpm stirs, collect the filtrate 4.2kg that weighs, the gac that adds 440g again is as discoloring agent, the rotating speed centrifuging of back with 1400rpm stirs, collect the polyoxyethylene glycol that filtrate obtains, and weigh.
(2) with washed with de-ionized water solid sand material, and dry; The sand material by magnetic grader, is removed the metal in the shakeout material, obtain the mixture of silicon and silicon carbide.
(3) pouring the mixture of the silicon of step (2) and silicon carbide into internal surface has in the quartz crucible of silicon nitride layer; The crucible that the sand material is housed is changed in the vacuum resistance furnace over to 1450 ℃ of heating 3h; After being cooled to room temperature, cross the screen cloth of 200 μ m, collect silico briquette on the sieve, sieve is collected silicon carbide micro-powder down, and weigh.
(4) will sieve the silico briquette of collecting and change in the micronizer mill, 0.7MPa pulverizes 5min down, obtains silica flour, and weighs.
Comparative Examples 1
Adopt step (1) and (2) identical, obtain the mixture of silicon and silicon carbide, change in the settling centrifuge then with embodiment 1, pressurization 3bar, work 6h obtains silicon and silicon carbide respectively from the difference outlet, wash drying respectively and obtain silica flour, silicon carbide micro-powder, and weigh respectively.
Embodiment 2
Composition preparation waste mortar according to embodiment 1: cutting liquid 44wt%, silicon carbide micro-powder 48wt%, silica flour 6.8wt%, metallic particles 1.2wt%.
(1) with the rotating speed centrifugation 30min of 10Kg waste mortar, obtains liquid and solid sand material with 2000rpm.In liquid, add 440g polyacrylamide and 440g diatomite, the rotating speed centrifuging of back with 2000rpm stirs, collect the filtrate 3.9kg that weighs, the gac that adds 440g again is as discoloring agent, the rotating speed centrifuging of back with 2000rpm stirs, collect filtrate and obtain polyoxyethylene glycol, and weigh.
(2) with washed with de-ionized water solid sand material, and dry; The sand material by magnetic grader, is removed the metal in the shakeout material, obtain the mixture of silicon and silicon carbide.
(3) pouring the mixture of the silicon of step (2) and silicon carbide into internal surface has in the quartz crucible of silicon nitride layer; The crucible that the sand material is housed is changed in the vacuum resistance furnace over to 1500 ℃ of heating 3h; After being cooled to room temperature, cross the screen cloth of 150 μ m, collect silico briquette on the sieve, sieve is collected silicon carbide micro-powder down, and weigh.
(4) will sieve the silico briquette of collecting and change in the micronizer mill, 0.5MPa pulverizes 5min down, obtains silica flour, and weighs.
Comparative Examples 2
Adopt step (1) and (2) identical with embodiment 2, obtain the mixture of silicon and silicon carbide, change over to then in methenyl bromide-alcohol mixing solutions (density is 2.75g/mL), ultrasonic oscillation 10min, leave standstill 30min, collect the floating matter on the liquid, with hydrofluoric acid solution (5wt%) washing, drying, obtain silica flour, and weigh; Collect throw out in the liquid, washing, drying obtain silicon carbide micro-powder, and weigh.
The weighing results of embodiment 1-2 and Comparative Examples 1-2 is as shown in table 1.
Table 1
| Sample | Indicated weight | S1 | DS1 | S2 | DS2 |
| Polyoxyethylene glycol (kg) | 4.4 | 3.5 | 3.5 | 3.2 | 3.2 |
| Silicon carbide (kg) | 4.8 | 3.9 | 3.5 | 4.2 | 3.9 |
| Silica flour (kg) | 0.68 | 0.6 | 0.9 | 0.65 | 0.75 |
From the test result of last table 1 as can be seen, recovery method of the present invention, all higher to the rate of recovery of polyoxyethylene glycol, silicon carbide and silica flour.Wherein the result of S1 and DS1 still contains 32% silicon carbide in the silica flour that adopts gravitational segregation to reclaim more as can be seen, reduces the rate of recovery of silicon carbide on the one hand, and the purity of silica flour is lower on the other hand; The result of S2 and DS2 relatively finds out, also contains 10% silicon carbide in the silica flour of heavy-fluid flotation, has influenced the purity of the silica flour that reclaims.
Claims (7)
1. the recovery method of a silicon chip dicing waste mortar may further comprise the steps:
A. the silicon chip dicing waste mortar solid-liquid separation obtains solid sand material and liquid part;
B. add discoloring agent, ion adsorbent and flocculating aids in the liquid part that obtains among the step a, solid-liquid separation obtains the polyoxyethylene glycol cutting and reclaims liquid;
C. the solid sand material that obtains among the step a separates by magnetic separation removes metal, obtains the mixture of silicon and silicon carbide;
D. with the mixture of the silicon that obtains among the step c and silicon carbide 1425-1550 ℃ of following heating under vacuum; Be cooled to screen cloth vibration filtering after the room temperature, collect undersized material and obtain silicon carbide micro-powder, the material on the collection screen obtains silico briquette; Pulverize silico briquette and obtain silica flour.
2. recovery method according to claim 1 is characterized in that: among the step a, solid-liquid separation adopts centrifugation, and centrifugal rotational speed is 1000-2000rpm, centrifugation time 20-40min.
3. recovery method according to claim 1 is characterized in that: among the step b, discoloring agent is gac and/or ammonium persulphate, and ion adsorbent is polyacrylamide or Poly Dimethyl Diallyl Ammonium Chloride, and flocculating aids is diatomite or perlite; Mass ratio is liquid part: discoloring agent: ion adsorbent: flocculating aids=(10-5): 1: 1: 1.
4. recovery method according to claim 1 is characterized in that: in the steps d, the temperature of heating under vacuum is 1450-1480 ℃, and vacuum tightness is not higher than-0.01MPa; The time of heating under vacuum is 3-6h.
5. according to claim 1 or 4 described recovery methods, it is characterized in that: in the steps d, the heating under vacuum process of the mixture of silicon and silicon carbide is carried out in crucible; Described crucible internal layer surface is covered with silicon nitride layer, and crucible body material is quartz or alumina-ceramic.
6. according to claim 1 or 4 described recovery methods, it is characterized in that: in the steps d, screen mesh size is the 100-300 order, and the screen cloth vibrational frequency is 40-80 time/min.
7. recovery method according to claim 1 is characterized in that: in the steps d, the method for pulverizing silico briquette is a comminution by gas stream, and stream pressure is 0.5-0.7MPa; The time of comminution by gas stream is 5-20min.
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| CN102757856A (en) * | 2012-07-30 | 2012-10-31 | 江苏阳帆机电设备制造有限公司 | Online recovery method for waste mortar produced in silicon wafer cutting |
| CN102977990A (en) * | 2012-11-16 | 2013-03-20 | 晶科能源有限公司 | Circulation process of distilled water in recycling process of silicon cutting fluids |
| CN103072989A (en) * | 2013-01-09 | 2013-05-01 | 烟台同立高科新材料股份有限公司 | Method for recycling boron carbide in sapphire polishing waste slurry |
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| CN103183349A (en) * | 2011-12-31 | 2013-07-03 | 浙江昱辉阳光能源有限公司 | Recovery method for silicon carbide and polyethyleneglycol cutting fluids in waste cutting mortar for silicon wafer |
| CN104120026A (en) * | 2014-08-07 | 2014-10-29 | 佳明新材料科技有限公司 | Method for comprehensively recycling SiC cutting fluid waste mortar |
| 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 |
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| CN103183349B (en) * | 2011-12-31 | 2015-03-11 | 浙江昱辉阳光能源有限公司 | Recovery method for silicon carbide and polyethyleneglycol cutting fluids in waste cutting mortar for silicon wafer |
| CN103183349A (en) * | 2011-12-31 | 2013-07-03 | 浙江昱辉阳光能源有限公司 | Recovery method for silicon carbide and polyethyleneglycol cutting fluids in waste cutting mortar for silicon wafer |
| CN102757856B (en) * | 2012-07-30 | 2013-10-09 | 江苏阳帆机电设备制造有限公司 | Online recovery method for waste mortar produced in silicon wafer cutting |
| CN102757856A (en) * | 2012-07-30 | 2012-10-31 | 江苏阳帆机电设备制造有限公司 | Online recovery method for waste mortar produced in silicon wafer cutting |
| CN102977990A (en) * | 2012-11-16 | 2013-03-20 | 晶科能源有限公司 | Circulation process of distilled water in recycling process of silicon cutting fluids |
| CN103072989A (en) * | 2013-01-09 | 2013-05-01 | 烟台同立高科新材料股份有限公司 | Method for recycling boron carbide in sapphire polishing waste slurry |
| CN103072988A (en) * | 2013-01-09 | 2013-05-01 | 烟台同立高科新材料股份有限公司 | Method for recycling boron carbide in sapphire grinding waste slurry |
| CN103072989B (en) * | 2013-01-09 | 2014-07-09 | 烟台同立高科新材料股份有限公司 | Method for recycling boron carbide in sapphire polishing waste slurry |
| CN103072988B (en) * | 2013-01-09 | 2014-07-16 | 烟台同立高科新材料股份有限公司 | Method for recycling boron carbide in sapphire grinding waste slurry |
| 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 |
| CN104120026A (en) * | 2014-08-07 | 2014-10-29 | 佳明新材料科技有限公司 | Method for comprehensively recycling SiC cutting fluid waste mortar |
| CN105001969A (en) * | 2015-07-07 | 2015-10-28 | 阳光硅峰电子科技有限公司 | Highly efficient mortar separation method based on temperature sensitivity |
| CN105001969B (en) * | 2015-07-07 | 2017-12-01 | 阳光硅峰电子科技有限公司 | A kind of method for efficiently separating mortar based on temperature sensitivity |
| CN105924771A (en) * | 2016-05-12 | 2016-09-07 | 安徽理工大学 | Polypropylene material modified with photovoltaic crystal silicon processing waste and preparation method of polypropylene material |
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| CN116177552B (en) * | 2023-02-22 | 2023-11-17 | 江苏秉盛环保工程有限公司 | Silicon wafer cutting fluid silicon powder recovery system and process thereof |
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