CN101244823B - Method for recycling silicon carbide from by-product in silicon slice cutting process - Google Patents
Method for recycling silicon carbide from by-product in silicon slice cutting process Download PDFInfo
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Abstract
The invention relates to a method of recovering silicon carbide from the byproducts of the cut processing of solar-grade silicon wafer and electronic-grade wafer. Concretely speaking, in the wafer cut processing, a large amount of slurry cutting liquid is required to be added to reduce mechanical stress and heat stress and make linear cutting process a stable process; thus, a large amount of byproducts comprising a great amount of organic compounds, silicon carbide and polysilicon (moncrystalline silicon) are made; the silicon carbide powder used for the cutting processing of silicon wafer can be recovered from the byproducts. According to the technical proposal provided by the invention, after separation agent is added into silicon wafer cutting byproducts, the sizing agent rich in silicon carbide can be obtained after mechanical separation; after second mechanical separation, the wet solid, after the processes of alkali cleaning, pickling, rinsing, mechanical separation, drying and size classification, can get the silicon carbide powder which can be used for the cutting processing of silicon wafer.
Description
Technical field
The present invention relates to a kind of method that from silicon chip cutting processing by product, reclaims silicon carbide.Application Areas mainly is sun power industry silicon chip cutting processing by product, electron trade silicon chip cutting processing by product.Reclaim the cutting processing that high-purity carborundum can be back to silicon chip, also can be used for the place that other commodity silicon carbide is suitable for.
Background technology
In order to reduce mechanical stress, thermal stresses, the security system cutting process becomes stable process in the silicon chip cutting processing process, needs to add a large amount of cutting liquid, can produce a large amount of by products in the course of processing.The main component of this by product is that large amount of organic (promptly cuts the main component of liquid: the mixed solution of ethylene glycol, many ethylene glycol, ethylene glycol monomethyl ether, tensio-active agent), and when using this cutting liquid, be added on silicon carbide (this silicon carbide is as the abrasive material that cuts liquid) wherein and polysilicon (or silicon single crystal) particle that in cutting process, produces.Silicon chip cutting processing by product not only can produce serious environmental and pollute, and waste a large amount of resources if deal with improperly.Along with country is energy-saving and cost-reducing, the higher silicon carbide of economic worth is reclaimed in the enforcement of protection Environmental policy from silicon chip cutting processing by product, can be back to the cutting processing process of silicon chip, also can be used for the use occasion of commodity silicon carbide.
Silicon carbide has two kinds of crystal formations, and β-type is a cubes, α=0.4350nm ultrahard.Green to black-and-blue.Specific inductivity 7.Hardness 9Mobs.A-is a semi-conductor.Mobility (300K), cm
2/ (VS), 400 electronics and 50 holes, bands of a spectrum gap eV, 303 (0K) and 2.996 (300K); Virtual mass 0.60 electronics and 1.00 holes, electric conductivity, pyro-oxidation resistance.Relative density 3.16.2830 ℃ of fusing points.Thermal conductivity (500 ℃) 22.5, (1000 ℃) 23.7W/ (m
2K).Thermal expansivity: linear in 100 ℃: 5.2 * 10
-6/ ℃, water insoluble, pure; Be dissolved in molten alkali hydroxide.Usually silicon carbide is in the cutting processing process, because mechanical force causes spherical coefficient, particle diameter and the size distribution of silicon-carbide particles to change; In addition, in the use of cutting liquid, the powder that polysilicon is cut and other mechanical impurity mix in wherein, form Combination cutting processing by product.The cutting exigent purity of silicon-carbide particles and certain spherical coefficient, suitable size distribution.So, silicon chip cutting processing by product can not direct reuse in production process.Silicon carbide is as important material, because the production process complexity consumes a large amount of energy, the price height is so people are devoted to the silicon carbide micro-powder that extracts high purity from silicon chip cutting processing by product, meet silicon chip cutting processing processing requirement always.
The objective of the invention is to study and a kind ofly from silicon chip cutting processing by product, extract high purity, meet the method for the silicon-carbide particles of silicon chip cutting processing processing requirement.
Summary of the invention
The objective of the invention is to study a kind of method of from solar energy-level silicon wafer cutting processing by product, electronic-grade silicon chip cutting processing by product, extracting the high-purity carborundum particulate.
According to technical scheme provided by the invention, silicon chip cutting processing by product adds separating agent after mixing, and consumption is 5～50%, and mixing temperature is a normal temperature or 50 ℃～80 ℃ (improving temperature can raise the efficiency); Send into mechanical separator with transmission machinery, the service temperature of mechanical separator is 5～80 ℃; By the rich silicon carbide slurry of mechanical separator acquisition 50～95% and 5～50% poor silicon carbide suspension; Rich silicon carbide slurry carries out multi-stage mechanical again to be separated, and the high-purity carborundum slurry of acquisition is removed cutting liquid and separating agent by mechanical separation again, carries out alkali cleaning, pickling and cleaning then, after gained silicon carbide wet feed drying, the classification, gets the high-purity carborundum product.
Comprise solar energy-level silicon wafer cutting processing by product and electronic-grade silicon chip cutting processing by product in the silicon chip cutting processing by product.
The silicon carbide that reclaims is used for silicon chip cutting processing process or as silicon carbide products; Described poor silicon carbide suspension by agent of mechanical separation extraction separation and cutting liquid, reclaims polysilicon as later process.
Before rich silicon carbide slurry being carried out the multi-stage mechanical separation, in rich silicon carbide slurry, add separating agent once more.Described separating agent comprises one or more the mixture in the following substances:
One or more mixed solutions in the polyoxyethylene glycol of a, ethylene glycol, Diethylene Glycol, triethylene glycol, molecular-weight average 200～10000Dalton;
B, nonionogenic tenside;
One or more mixtures in c, polyethylene glycol monooleate, polyoxyethylene glycol dioleic acid ester, polyethylene glycol mono stearate, the Triglycol distearate;
D, secondary alkyl ethoxylated (JFC) permeate agent of polyoxyethylene;
E, viscosity-controlling agent, the main component of this viscosity-controlling agent is for containing polyhydric polyacrylic ester.
Mechanical separator comprises the one or more combination in settling bowl, scraper plate settling vessel, inclined plate settler, horizontal centrifuge, vertical centrifugal machine, tubular-bowl centrifuge and the swirler.
The used alkali of alkali cleaning is the metal hydroxides of liquid or solid, and the alkali cleaning temperature is a normal temperature or at 50 ℃～120 ℃; The used acid of pickling is mineral acid or organic acid, perhaps the mixture of organic acid and mineral acid; Described acid is pure acid or acid solution, and temperature is a normal temperature or at 50 ℃～120 ℃; With clean clear water, cleaning temperature is 50～120 ℃, obtains the silicon carbide wet feed through mechanical separation again after cleaning during cleaning.
Used furnace drying method comprises when oven dry silicon carbide wet feed: fluid-bed drying, fixed bed drying method; 40～150 ℃ of bake out temperatures, oven dry pressure comprises constant pressure and dry and vacuum-drying; Described stage division comprises: method of sieving and the classification of air-flow method.
Described ethylene glycol comprises one or more mixed solutions in ethylene glycol monomethyl ether, glycol dimethyl ether, ethylene glycol monoethyl ether, ethylene glycol bis ether, the ethylene glycol monobutyl ether;
Described metal hydroxides is sodium hydroxide, potassium hydroxide or yellow soda ash; Described mineral acid is sulfuric acid, carbonic acid, nitric acid, hydrochloric acid; Described organic acid is oxalic acid, citric acid.
Advantage of the present invention is: silicon chip cutting processing by product is processed, can be obtained to satisfy the silicon carbide micro-powder that the silicon chip cutting processing requires, and provide condition for cutting liquid reclaims, resource is fully used, reduce the pollution to environment.
Embodiment
Silicon chip cutting processing by product is earlier through pre-treatment, remove contained large granular impurity, enter mixing equipment, after mechanical stirring is even, add polyoxyethylene glycol, diethylene glycol ether, ethylene glycol monomethyl ether, tensio-active agent, permeate agent, polyethylene glycol (PEG) oleate, viscosity-controlling agent etc., stir down at normal temperature or 50 ℃～80 ℃ (improving temperature can raise the efficiency), purpose is to make each component formation better physical effect and chemical action in graininess solids and the mixed solution.Finely disseminated suspension is sent into separating machine, and separating machine comprises the one or more combination in settling bowl, scraper plate settling vessel, inclined plate settler, horizontal centrifuge, vertical centrifugal machine, tubular-bowl centrifuge and the swirler etc.; The operation of separating machine can intermittent type, continous way or intermittently and continuous hybrid operation; Be separated into slurry and the poor silicon carbide suspension that is rich in silicon carbide through normal temperature or at 50 ℃～80 ℃ (improving temperature can raise the efficiency) separating machines.Separating obtained rich silicon carbide slurry is 50～95% for the first time, poor silicon carbide suspension 5～50%; The poor silicon carbide suspension of gained can be carried out organism and be reclaimed.The rich silicon carbide slurry of gained adds above-mentioned each component once more, after mixing, carries out separating machine and separates, and it can be 1～5 time that separating machine separates number of times.The separating obtained poor silicon carbide suspension of stage trapping machine can be used for the primary separation machine and separate, and maybe can be used for fluid organic material and separate, or remove the organism recovery process.The slurry that gained contains high density carbonization silicon washs, or washs after separating liquid wherein.Alkali cleaning is carried out in washing earlier, alkali cleaning can be liquid caustic soda or solid alkali, alkali is metal hydroxidess such as NaOH, KOH, wash temperature is a normal temperature or 50 ℃～120 ℃ (improve temperature can raise the efficiency), after the alkali cleaning, carry out pickling behind the separating liquid, pickling is mineral acid or organic acids such as oxalic acid, citric acid such as sulfuric acid, carbonic acid, nitric acid, hydrochloric acid, the perhaps mixture of organic acid and mineral acid, acid can be pure acid or solution, and temperature is a normal temperature or 50 ℃～120 ℃ (improve temperature can raise the efficiency).After separating removal liquid after the pickling, extremely neutral with water rinse.The rinsing temperature is a normal temperature or 50 ℃～120 ℃ (improve temperature can raise the efficiency).After separating once more, hygrometric state silicon carbide is carried out drying.Drying can be used fixed bed drying device or fluidized bed dryer; The drying pressure pattern can be normal pressure, pressurization or vacuum-drying, and the silicon carbide of drying is sieved, and obtains the silicon carbide micro-powder of different purposes according to screening.
Embodiment 1
Get the sample 1000g of silicon chip cutting by product, add the flask that band stirs, after stirring, add the 250g separating agent, mixing temperature is a normal temperature or at 50～80 ℃, consisting of of separating agent: Macrogol 200 (PEG200) 50g, cetomacrogol 1000 0 (PEG10000) 20g, polyethyleneglycol ether 12g, polyethylene glycol monooleate (DO400) 5g, nonionogenic tenside (OP-10) 11g, permeate agent (JFC) 8g, after stirring under 5 ℃, enter separating centrifuge, obtain rich silicon carbide slurry of 750g and poor silicon carbide suspension 500g, rich silicon carbide slurry after the secondary centrifugation, is rich in silicon carbide slurry and stirs 1h with 25%NaOH solution down at 50 ℃, enter separating centrifuge, after removing most of liquid, add again 70% sulfuric acid 50 ℃ down stir 1h after, enter separating centrifuge, remove most of liquid after, use the clear water rinsing to neutral again, after mechanical separation, in 80 ℃ of following oven drying 8h, dried powder obtains product with method of sieving, join solar silicon wafers cutting liquid to solar level silicon rod line cutting processing with fresh silicon carbide with 6: 4 ratios, satisfy the requirement of complete processing.
Embodiment 2
Get the sample 1000g of silicon chip cutting by product, add the flask that band stirs, after stirring, add the 350g separating agent, consisting of of separating agent: Macrogol 200 (PEG200) 100g, cetomacrogol 1000 0 (PEG10000) 50g, polyethyleneglycol ether 22g, polyethylene glycol monooleate (DO400) 8g, polyoxyethylene glycol dioleic acid ester (MO600) 8g nonionogenic tenside (OP-10) 12g, permeate agent (JFC) 8g, after stirring under 80 ℃, enter separating centrifuge, obtain rich silicon carbide slurry of 800g and poor silicon carbide suspension 453g, to rich silicon carbide slurry after the secondary centrifugation, be rich in silicon carbide slurry and stir 1h down at 50 ℃ with 30%NaOH solution, enter separating centrifuge, remove most of liquid after, add again 60% sulfuric acid 50 ℃ stir 1h down after, enter separating centrifuge, after removing most of liquid, use the clear water rinsing again to neutral, after mechanical separation, in 80 ℃ of following oven drying 8h, dried powder obtains product with method of sieving, joins solar silicon wafers cutting liquid to solar level silicon rod line cutting processing with fresh silicon carbide with 7: 3 ratios, satisfies the requirement of complete processing.
Embodiment 3
Get the sample 1000g of silicon chip cutting by product, add the flask that band stirs, after stirring, add the 200g separating agent, consisting of of separating agent: poly(oxyethylene glycol) 400 (PEG400) 50g, polyoxyethylene glycol 800 (PEG800) 20g, polyethyleneglycol ether 12g, polyethylene glycol monooleate (DO400) 5g, polyoxyethylene glycol dioleic acid ester (MO600) 5g nonionogenic tenside (OP-10) 8g, permeate agent (JFC) 8g, viscosity-controlling agent 5g is after stirring under 40 ℃, enter separating centrifuge, obtain rich silicon carbide slurry of 813g and poor silicon carbide suspension 528g, to rich silicon carbide slurry after the secondary centrifugation, be rich in silicon carbide slurry and stir 1h down at 50 ℃ with 30%NaOH solution, enter separating centrifuge, remove most of liquid after, add again 60% nitric acid 50 ℃ down stir 1h after, enter separating centrifuge, after removing most of liquid, use the clear water rinsing again to neutral, after mechanical separation, in 80 ℃ of following oven drying 8h, dried powder obtains product with method of sieving, joins solar silicon wafers cutting liquid to solar level silicon rod line cutting processing with fresh silicon carbide with 5: 5 ratios, satisfies the requirement of complete processing.
Embodiment 4
Get the sample 1000g of silicon chip cutting by product, add the flask that band stirs, after stirring, add the 300g separating agent, consisting of of separating agent: poly(oxyethylene glycol) 400 (PEG400) 92g, polyoxyethylene glycol 800 (PEG800) 50g, polyethyleneglycol ether 15g, polyethylene glycol monooleate (DO400) 10g, polyoxyethylene glycol dioleic acid ester (MO600) 12g, nonionogenic tenside (OP-10) 14g, permeate agent (JFC) 10g, viscosity-controlling agent 5g is after stirring under 60 ℃, enter separating centrifuge, obtain rich silicon carbide slurry of 803g and poor silicon carbide suspension 500g, rich silicon carbide slurry after three grades of centrifugations, is rich in silicon carbide slurry and stirs 1h with 30%NaOH solution down at 50 ℃, enter separating centrifuge, after removing most of liquid, add again 60% nitric acid 50 ℃ down stir 1h after, enter separating centrifuge, remove most of liquid after, use the clear water rinsing to neutral again, after mechanical separation, in 80 ℃ of following oven drying 8h, dried powder obtains product with method of sieving, join solar silicon wafers cutting liquid to solar level silicon rod line cutting processing with fresh silicon carbide with 8: 2 ratios, satisfy the requirement of complete processing.
Claims (10)
1. method that from silicon chip cutting processing by product, reclaims silicon carbide, it is characterized in that: silicon chip cutting processing by product is after mixing, add separating agent, consumption is 5～50% of a silicon chip cutting processing by product, and mixing temperature is a normal temperature or at 50～80 ℃; Send into mechanical separator with transmission machinery, the service temperature of mechanical separator is 5～80 ℃; By the rich silicon carbide slurry of mechanical separator acquisition 50～95% and 5～50% poor silicon carbide suspension; Rich silicon carbide slurry carries out multi-stage mechanical again to be separated, and the high-purity carborundum slurry of acquisition is removed cutting liquid and separating agent by mechanical separation again, carries out alkali cleaning, pickling and cleaning then, after gained silicon carbide wet feed drying, the classification, gets the high-purity carborundum product;
Described separating agent comprises one or more the mixture in the following substances:
The polyoxyethylene glycol of a, ethylene glycol, Diethylene Glycol, triethylene glycol, molecular-weight average 200～10000Dalton;
B, nonionogenic tenside;
C, viscosity-controlling agent, the main component of this viscosity-controlling agent is for containing polyhydric polyacrylic ester.
2. according to the described method of claim 1, it is characterized in that: comprise solar energy-level silicon wafer cutting processing by product and electronic-grade silicon chip cutting processing by product in the silicon chip cutting processing by product from silicon chip cutting processing by-product recovery silicon carbide.
3. according to the described method from silicon chip cutting processing by-product recovery silicon carbide of claim 1, it is characterized in that: the silicon carbide of recovery is used for silicon chip cutting processing process or as silicon carbide products; Described poor silicon carbide suspension by agent of mechanical separation extraction separation and cutting liquid, reclaims polysilicon as later process.
4. according to the described method of claim 1, it is characterized in that: before rich silicon carbide slurry being carried out the multi-stage mechanical separation, in rich silicon carbide slurry, add separating agent once more from silicon chip cutting processing by-product recovery silicon carbide.
5. according to the described method of claim 1, it is characterized in that described nonionogenic tenside is from silicon chip cutting processing by-product recovery silicon carbide:
One or more mixtures in polyethylene glycol monooleate, polyoxyethylene glycol dioleic acid ester, polyethylene glycol mono stearate, the Triglycol distearate;
Or the secondary alkyl ethoxylated permeate agent of polyoxyethylene.
6. according to the described method from silicon chip cutting processing by-product recovery silicon carbide of claim 1, it is characterized in that: mechanical separator comprises the one or more combination in settling bowl, scraper plate settling vessel, inclined plate settler, horizontal centrifuge, vertical centrifugal machine, tubular-bowl centrifuge and the swirler.
7. according to the described method from silicon chip cutting processing by-product recovery silicon carbide of claim 1, it is characterized in that: the used alkali of alkali cleaning is the metal hydroxides of liquid or solid, and the alkali cleaning temperature is a normal temperature or at 50 ℃～120 ℃; The used acid of pickling is mineral acid or organic acid, perhaps the mixture of organic acid and mineral acid; Described acid is pure acid or acid solution, and temperature is a normal temperature or at 50 ℃～120 ℃; With clean clear water, cleaning temperature is 50～120 ℃, obtains the silicon carbide wet feed through mechanical separation again after cleaning during cleaning.
8. according to the described method of claim 1, it is characterized in that used furnace drying method comprises when oven dry silicon carbide wet feed: fluid-bed drying, fixed bed drying method from silicon chip cutting processing by-product recovery silicon carbide; 40～150 ℃ of bake out temperatures, oven dry pressure comprises constant pressure and dry and vacuum-drying; Described stage division comprises: method of sieving and the classification of air-flow method.
9. according to the described method of claim 1 from silicon chip cutting processing by-product recovery silicon carbide, it is characterized in that described separating agent also comprises one or more mixed solutions in ethylene glycol monomethyl ether, glycol dimethyl ether, ethylene glycol monoethyl ether, ethylene glycol bis ether, the ethylene glycol monobutyl ether;
10. according to the described method of claim 7, it is characterized in that described metal hydroxides is sodium hydroxide or potassium hydroxide from silicon chip cutting processing by-product recovery silicon carbide; Described mineral acid is sulfuric acid, carbonic acid, nitric acid or hydrochloric acid; Described organic acid is oxalic acid or citric acid.
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| CN104316433A (en) * | 2014-11-17 | 2015-01-28 | 江南大学 | Analytic method for measuring component content of waste mortar during silicon cutting |
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