CN101804983A - Recovery, purification and classification method of high-purity silicon carbide micro-powder - Google Patents
Recovery, purification and classification method of high-purity silicon carbide micro-powder Download PDFInfo
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Abstract
The invention relates to a recovery, purification and classification method of high-purity silicon carbide micro-powder. The method for realizing recovery, purification and classification of high-purity silicon carbide micro-powder based on cutting of a silicon wafer and machining of mortar comprises the following steps: step 1: adding flocculating agent of which the dosage is 0.1%-10% in the processes of cutting of the silicon wafer and machining of the mortar for accelerating precipitation, and filtering to obtain a solid matter; step 2: carrying out alkali cleaning, acid cleaning and cleaning on the solid matter to obtain silicon carbide slurry; step 3: adding dispersing agent of which the dosage is 0.1%-20% into the silicon carbide slurry; and step 4: carrying out hydraulic classification by using a suspension method through a classification and screening device to control classification, control water flow and collect overflow micro-powder, and drying to obtain high-purity silicon carbide products of different specifications and particle sizes. The technical method for recovery, purification and classification is simple and convenient and has strong controllability, the silicon carbide products have centralized particles and uniform particle size distribution, and the method has low requirements for equipment investment environment and low operating cost for industrialized implementation and is convenient for large-scale industrialized implementation.
Description
Technical field
A kind of recovery purification and stage division of high-purity silicon carbide micro-powder.Its Application Areas mainly realizes the high-purity silicon carbide micro-powder resource utilization from silicon slice cutting and processing mortar.
Technical background
Silicon carbide Silicon Carbide is abbreviated as SiC.Molecular formula: SiC.Silicon carbide is crystal, the hardness height, and cutting power is stronger, and the chemical ability is stable, good heat conductivity.Microhardness 3,280～3,400kg/mm
2Can make fixed and coated abrasive tool, cutting, free grinding and polishing etc.; Be fit to processing rigid alloy, rapid steel etc.; But non-metallic material such as abrading glass, pottery, stone material, semi-conductor, agate and senior jewelry jade object also.
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 process such as the silicon chip cutting processing, can use a large amount of cutting fluids simultaneously, powder and other mechanical impurity that the while crystal silicon is cut also can be mixed in together, thereby form Combination cutting processing by product, usually are referred to as mortar (or waste mortar).
Solids in the silicon slice cutting and processing mortar is analyzed, wherein the component that must comprise:
1, SiC particle (normal size)
2, SiC particle (normal size is coated with metal fine powder)
3, SiC particle (normal size is coated with silicon powder)
4, SiC particle (normal size is coated with metal fine powder and silicon powder)
5, SiC particle (less than normal size)
6, metal fine powder
7, silicon powder
Silicon chip the cutting processing exigent purity of silicon-carbide particles and certain spherical coefficient, suitable size distribution.So the direct reuse that the silicon carbide in the mortar can not be easy is in the cutting production process of silicon chip.Silicon carbide is as important material, because the production process complexity consumes a large amount of energy, the price height, so people are devoted to realize the high-purity silicon carbide micro-powder resource utilization from silicon slice cutting and processing mortar, extract highly purified, as to meet silicon chip cutting processing processing requirement silicon carbide micro-powder always.
The object of the present invention is to provide a kind of from silicon slice cutting and processing mortar the recovery purification and the stage division of silicon carbide micro-powder.
Summary of the invention
The invention provides a kind of recovery purification and stage division of high-purity silicon carbide micro-powder.Based on silicon slice cutting and processing mortar, realize that high-purity silicon carbide micro-powder reclaims purification and the fractionated step comprises:
Step 1: add flocculation agent to quicken sedimentation in silicon slice cutting and processing mortar, consumption is 0.1%-10%, obtains solids after filtration;
Step 2: solids is carried out alkali cleaning, pickling and cleaning, obtain silicon carbide slurry;
Step 3: in silicon carbide slurry, add dispersion agent, consumption 0.1%-20%;
Step 4: by classification, branch device, carry out the suspension method hydraulic classification, controlling classification control discharge is collected the overflow micro mist, and drying obtains the high-purity carborundum product of different size and size composition.
Described silicon slice cutting and processing mortar comprises solar energy-level silicon wafer cutting and machining mortar and electronic-grade silicon chip cutting and machining mortar.
Described flocculation agent comprises polymerize aluminum chloride, the one or more combination in polyaluminium sulfate, bodied ferric sulfate, active silicic acid, composite flocculation agent, non-ionic type organic polymer coargulator, anionic organic polymer coargulator, cationic organic polymer coargulator, amphiprotic polyacrylamide polymkeric substance, acrylamide grafted copolymer, the microbial flocculant.
The used alkali of described alkali cleaning is the metal hydroxides of liquid or solid; 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; Use clean clear water during cleaning.Metal hydroxides described herein is sodium hydroxide, potassium hydroxide or yellow soda ash; Described mineral acid is sulfuric acid, carbonic acid, nitric acid, hydrochloric acid, hydrofluoric acid; Described organic acid is acetic acid, oxalic acid, citric acid.
By alkali cleaning, pickling and cleaning main purpose is silicon powder, the metal fine powder of removing silicon powder, metal fine powder and being wrapped in the SiC particle surface.Mainly contain the SiC particle of normal size and, have very high purity through the silicon carbide slurry after alkali cleaning, pickling and the cleaning less than the SiC particle of normal size.
Described dispersion agent comprises one or more in water glass, tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, trisodium phosphate, triethyl hexyl phosphoric acid, sodium lauryl sulphate, methyl amyl alcohol, derivatived cellulose, polyacrylamide, guar gum, the fatty acid polyglycol ester.
Described classification, branch device comprise the one or more combination in classification jar, classification still, tank classifier, branch machine, the sifting machine.
The water that is adopted in the described suspension method hydraulic classification is the water through processing, specific conductivity≤200 μ S/cm.
Described controlling classification control discharge is collected the overflow micro mist, classification, branch device according to different size, according to discharge operational procedure from small to large, set and adjust according to suspension method hydraulic classification process size composition analysis situation of collected overflow micro mist under particular water amount situation.
Described furnace drying method comprises: fluid-bed drying, fixed bed drying method; 40～150 ℃ of bake out temperatures, oven dry pressure comprises constant pressure and dry and vacuum-drying.
Embodiment
Explanation realizes that from silicon slice cutting and processing mortar high-purity silicon carbide micro-powder reclaims purification and fractionated method, specifically may further comprise the steps:
(1) silicon slice cutting and processing mortar is added flocculation agent to quicken sedimentation at settling tank, consumption is 1-10%, through after mixing, filters and obtains solids.The flocculation agent that is adopted can be a polymerize aluminum chloride, one or more in polyaluminium sulfate, bodied ferric sulfate, active silicic acid, composite flocculation agent, non-ionic type organic polymer coargulator, anionic organic polymer coargulator, cationic organic polymer coargulator, amphiprotic polyacrylamide polymkeric substance, acrylamide grafted copolymer, the microbial flocculant.
(2) solids is sent into the alkali cleaning pond, alkali cleaning can be liquid caustic soda or solid alkali, and alkali is NaOH, and metal hydroxidess such as KOH fully soak, stir.The purpose of alkali cleaning is to remove the silicon powder of the silicon powder that contains in the solids and SiC particle surface parcel, during produce a large amount of gases, system temperature raises automatically, controlled temperature is below 50 ℃, the agitator treating time is 1～2 hour.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, and acid can be pure acid or solution, temperature is a normal temperature.The purpose of pickling is to remove the metal fine powder that contains metal fine powder and SiC particle surface parcel in the solids, during produce a small amount of gas, the pickling agitator treating time is 1～2 hour.After separating removal liquid after the pickling, extremely neutral with the clear water rinsing of cleaning.
(3) through in silicon carbide slurry, adding dispersion agent, consumption 0.1%-20% after cleaning.The dispersion agent that is adopted can be one or more in water glass, tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, trisodium phosphate, triethyl hexyl phosphoric acid, sodium lauryl sulphate, methyl amyl alcohol, derivatived cellulose, polyacrylamide, guar gum, the fatty acid polyglycol ester.Fully stir to guarantee that silicon carbide micro-powder is fully disperseed.
(4) by classification, branch devices such as classification jar, classification still, tank classifier, branch machine, sifting machines, carry out the suspension method hydraulic classification.Institute's water need be treated, specific conductivity≤200 μ S/cm.Control discharge is collected the overflow micro mist, checks the size composition situation of collected micro mist, resulting classification micro mist is dried the high-purity carborundum product that obtains different size and size composition.The furnace drying method that is adopted comprises: fluid-bed drying, fixed bed drying method; 40～150 ℃ of bake out temperatures, oven dry pressure comprises constant pressure and dry and vacuum-drying.
Embodiment 1:
Utilization realizes that from silicon slice cutting and processing mortar high-purity silicon carbide micro-powder reclaims purification and classification, and the mass ratio of silicon carbide is 45% in the silicon slice cutting and processing mortar, and used silicon carbide is from Lianyungang Jiayu Electron Material Science Co., Ltd.Its concrete steps are as follows:
Step 1 is sent into silicon slice cutting and processing mortar 1000Kg in the settling tank by transferpump, opens and stirs after 10 minutes, in 20 minutes, add 5Kg amphiprotic polyacrylamide polymkeric substance, continue to stir 1 hour, left standstill 3 hours, carry out centrifugation by separating centrifuge and obtain solids.
Step 2 is transferred to the gained solid formation in the alkali cleaning pond, slowly adds 10%NaOH solution, slowly open to stir, and stirs 0.5h, during have a large amount of gases to emit, enter separating centrifuge, remove most of liquid after; Add 20% hydrochloric acid again, stir 0.5h after, enter separating centrifuge, remove most of liquid after; Use the clear water rinsing to neutral again.
Step 3 adds the 5Kg tripoly phosphate sodium STPP at above-mentioned silicon carbide slurry through machinery, fully stirs and checks that silicon carbide micro-powder is fully disperseed.
Step 4, to obtain abundant dispersive silicon carbide slurry pumps in the classification jar, introducing water with the time stage pot bottom upwards flows, control discharge is at 100-200L/h, after classification jar water is full, the size that upflow tube flows out silicon carbide micro-powder in the inspection keeps the current elution time at 6-12 hour below 5 μ m.After treating that above-mentioned superfine silicon carbide micro powder is told, increase discharge (200-500L/h), reexamine the normal distribution of the micro mist size of upflow tube at 5 μ m～24 μ m, D50 is at 11 μ m～12 μ m.Continue the current process, up to being classified as end.The silicon carbide micro-powder that classification is collected is respectively at fixed bed drying device constant pressure and dry 4h, the high-purity silicon carbide micro-powder 390Kg that obtains superfine silicon carbide micro powder 32Kg respectively and can be used for the silicon chip cutting processing.
Embodiment 2:
Utilization realizes that from silicon slice cutting and processing mortar high-purity silicon carbide micro-powder reclaims purification and classification, and the mass ratio of silicon carbide is 50% in the silicon slice cutting and processing mortar, and used silicon carbide is from Lianyungang Jiayu Electron Material Science Co., Ltd.Its concrete steps are as follows:
Step 1 is sent into silicon slice cutting and processing mortar 1000Kg in the settling tank by transferpump, opens and stirs after 10 minutes, in 20 minutes, add the 8Kg sodium polyacrylate, continue to stir 1 hour, left standstill 3 hours, carry out centrifugation by separating centrifuge and obtain solids.
Step 2 is transferred to the gained solid formation in the alkali cleaning pond, slowly adds 10%NaOH solution, slowly open to stir, and stirs 0.5h, during have a large amount of gases to emit, enter separating centrifuge, remove most of liquid after; Add 20% hydrochloric acid again, stir 0.5h after, enter separating centrifuge, remove most of liquid after; Use the clear water rinsing to neutral again.
Step 3 adds 10Kg water glass at above-mentioned silicon carbide slurry through machinery, fully stirs and checks that silicon carbide micro-powder is fully disperseed.
Step 4, to obtain abundant dispersive silicon carbide slurry pumps in the branch machine, the water of the bottom of branch machine introducing simultaneously upwards flows, control discharge is at 200-400L/h, after classification jar water is full, the size that upflow tube flows out silicon carbide micro-powder in the inspection keeps the current elution time at 8-16 hour below 6.5 μ m.After treating that above-mentioned superfine silicon carbide micro powder is told, increase discharge (400-900L/h), reexamine the normal distribution of the micro mist size of upflow tube at 6.5 μ m～24 μ m, D50 is at 11.5 μ m～12.5 μ m.Continue the current process, up to being classified as end.The silicon carbide micro-powder that classification is collected is respectively at fixed bed drying device constant pressure and dry 4h, the high-purity silicon carbide micro-powder 415Kg that obtains superfine silicon carbide micro powder 55Kg respectively and can be used for the silicon chip cutting processing.
Claims (9)
1. the recovery purification and the stage division of a high-purity silicon carbide micro-powder.It is characterized in that, realize that based on silicon slice cutting and processing mortar high-purity silicon carbide micro-powder reclaims purification and the fractionated step comprises:
Step 1: add flocculation agent to quicken sedimentation in silicon slice cutting and processing mortar, consumption is 0.1%-10%, obtains solids after filtration;
Step 2: solids is carried out alkali cleaning, pickling and cleaning, obtain silicon carbide slurry;
Step 3: in silicon carbide slurry, add dispersion agent, consumption 0.1%-20%;
Step 4: by classification, branch device, carry out the suspension method hydraulic classification, controlling classification control discharge is collected the overflow micro mist, and drying obtains the high-purity carborundum product of different size and size composition.
2. according to the recovery purification and the stage division of the described a kind of high-purity silicon carbide micro-powder of claim 1, it is characterized in that: silicon slice cutting and processing mortar comprises solar energy-level silicon wafer cutting and machining mortar and electronic-grade silicon chip cutting and machining mortar.
3. according to the recovery purification and the stage division of the described a kind of high-purity silicon carbide micro-powder of claim 1, it is characterized in that, described flocculation agent comprises polymerize aluminum chloride, the one or more combination in polyaluminium sulfate, bodied ferric sulfate, active silicic acid, composite flocculation agent, non-ionic type organic polymer coargulator, anionic organic polymer coargulator, cationic organic polymer coargulator, amphiprotic polyacrylamide polymkeric substance, acrylamide grafted copolymer, the microbial flocculant.
4. according to the recovery purification and the stage division of the described a kind of high-purity silicon carbide micro-powder of claim 1, it is characterized in that the used alkali of described alkali cleaning is the metal hydroxides of liquid or solid; 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; Use clean clear water during cleaning.Metal hydroxides described herein is sodium hydroxide, potassium hydroxide or yellow soda ash; Described mineral acid is sulfuric acid, carbonic acid, nitric acid, hydrochloric acid, hydrofluoric acid; Described organic acid is acetic acid, oxalic acid, citric acid.
5. according to the recovery purification and the stage division of the described a kind of high-purity silicon carbide micro-powder of claim 1, it is characterized in that described dispersion agent comprises one or more in water glass, tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, trisodium phosphate, triethyl hexyl phosphoric acid, sodium lauryl sulphate, methyl amyl alcohol, derivatived cellulose, polyacrylamide, guar gum, the fatty acid polyglycol ester.
6. according to the recovery purification and the stage division of the described a kind of high-purity silicon carbide micro-powder of claim 1, it is characterized in that described classification, branch device comprise the one or more combination in classification jar, classification still, tank classifier, branch machine, the sifting machine.
7. according to the recovery purification and the stage division of the described a kind of high-purity silicon carbide micro-powder of claim 1, it is characterized in that the water that is adopted in the described suspension method hydraulic classification is the water through processing, specific conductivity≤200 μ S/cm.
8. according to the recovery purification and the stage division of the described a kind of high-purity silicon carbide micro-powder of claim 1, it is characterized in that, described controlling classification control discharge is collected the overflow micro mist, classification, branch device according to different size, according to discharge operational procedure from small to large, set and adjust according to suspension method hydraulic classification process size composition analysis situation of collected overflow micro mist under particular water amount situation.
9. according to the recovery purification and the stage division of the described a kind of high-purity silicon carbide micro-powder of claim 1, it is characterized in that described furnace drying method comprises: fluid-bed drying, fixed bed drying method; 40～150 ℃ of bake out temperatures, oven dry pressure comprises constant pressure and dry and vacuum-drying.
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Cited By (21)
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| CN101979483A (en) * | 2010-10-09 | 2011-02-23 | 辽宁奥克化学股份有限公司 | Method for improving dispersibility of silicon carbide mortar |
| CN102009977A (en) * | 2010-10-29 | 2011-04-13 | 临沭山田研磨材有限公司 | Special dispersant for hydraulic overflow classification for high-purity superfine silicon carbide micro powder for linear cutting and using method |
| CN102010785A (en) * | 2010-10-29 | 2011-04-13 | 临沂市凯祥硅粉有限公司 | Method for recovering silicon carbide micropowder and wire-cutting fluid from silicon slice wire-cutting processing waste mortar |
| CN102079520A (en) * | 2011-01-12 | 2011-06-01 | 虹京环保有限公司 | Recycling method of silicon carbide |
| CN102285653A (en) * | 2011-06-02 | 2011-12-21 | 江苏大阳光辅股份有限公司 | Method for removing carbon impurities in silicon carbide micropowder |
| CN102311115A (en) * | 2011-08-24 | 2012-01-11 | 江阴巨能微粉科技有限公司 | Preparation method of high-purity green silicon carbide micropowder |
| CN102559361A (en) * | 2010-11-30 | 2012-07-11 | Sanwa生物技术株式会社 | Processing Method Of Silicon Cutting Waste Liquid |
| CN102626954A (en) * | 2012-02-14 | 2012-08-08 | 上海五同机械制造有限公司 | Silicon wafer cutting method and cut scrap recycling method |
| CN102631991A (en) * | 2012-04-09 | 2012-08-15 | 江阴浩博科技有限公司 | Method for removing free carbon in SiC micro-powder |
| CN104263319A (en) * | 2014-08-29 | 2015-01-07 | 平顶山易成新材料有限公司 | Method for preparing cutting abrasive from silicon carbide recovered sand obtained after cutting of crystalline silicon |
| CN105597928A (en) * | 2016-03-21 | 2016-05-25 | 平顶山市国邦新材料有限公司 | Silicon carbide powder production system |
| CN105818287A (en) * | 2016-05-31 | 2016-08-03 | 上海纳晶科技有限公司 | Method for preparing high-purity submicron hydrated silica and silica microparticles in batch |
| CN105858602A (en) * | 2016-04-08 | 2016-08-17 | 北京科技大学 | Polycrystalline silicon cutting waste material treatment method |
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| CN109127559A (en) * | 2018-07-16 | 2019-01-04 | 淮安利泰碳化硅微粉有限公司 | A kind of silicon carbide micro-powder cleaning device and its cleaning method |
| CN110702490A (en) * | 2019-11-01 | 2020-01-17 | 上海申和热磁电子有限公司 | Method for purifying and analyzing silicon carbide in semiconductor slice waste liquid |
| CN110860223A (en) * | 2019-12-05 | 2020-03-06 | 南京工业大学东海先进硅基材料研究院 | Grading method of superfine silicon carbide micro powder with narrow particle size distribution |
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| CN101979483A (en) * | 2010-10-09 | 2011-02-23 | 辽宁奥克化学股份有限公司 | Method for improving dispersibility of silicon carbide mortar |
| CN101979483B (en) * | 2010-10-09 | 2013-02-27 | 辽宁奥克化学股份有限公司 | Method for improving dispersibility of silicon carbide mortar |
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| CN102079520A (en) * | 2011-01-12 | 2011-06-01 | 虹京环保有限公司 | Recycling method of silicon carbide |
| CN102285653B (en) * | 2011-06-02 | 2013-04-10 | 江苏大阳光辅股份有限公司 | Method for removing carbon impurities in silicon carbide micropowder |
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| CN102311115A (en) * | 2011-08-24 | 2012-01-11 | 江阴巨能微粉科技有限公司 | Preparation method of high-purity green silicon carbide micropowder |
| CN102626954A (en) * | 2012-02-14 | 2012-08-08 | 上海五同机械制造有限公司 | Silicon wafer cutting method and cut scrap recycling method |
| CN102631991A (en) * | 2012-04-09 | 2012-08-15 | 江阴浩博科技有限公司 | Method for removing free carbon in SiC micro-powder |
| CN104263319B (en) * | 2014-08-29 | 2015-12-02 | 平顶山易成新材料有限公司 | Silicon carbide after utilizing crystalline silicon to cut reclaims the method that sand prepares cutting abrasive material |
| CN104263319A (en) * | 2014-08-29 | 2015-01-07 | 平顶山易成新材料有限公司 | Method for preparing cutting abrasive from silicon carbide recovered sand obtained after cutting of crystalline silicon |
| CN105597928A (en) * | 2016-03-21 | 2016-05-25 | 平顶山市国邦新材料有限公司 | Silicon carbide powder production system |
| CN105597928B (en) * | 2016-03-21 | 2017-05-03 | 平顶山市国邦新材料有限公司 | Silicon carbide powder production system |
| CN105858602A (en) * | 2016-04-08 | 2016-08-17 | 北京科技大学 | Polycrystalline silicon cutting waste material treatment method |
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| CN106957714A (en) * | 2017-03-24 | 2017-07-18 | 中磁科技股份有限公司 | The reclaimer and method of neodymium iron boron cutting greasy filth |
| CN108285147A (en) * | 2018-03-23 | 2018-07-17 | 河南易成新能源股份有限公司 | The method that high-purity silicon powder is extracted from crystalline silicon mortar cutting waste material |
| CN109127559A (en) * | 2018-07-16 | 2019-01-04 | 淮安利泰碳化硅微粉有限公司 | A kind of silicon carbide micro-powder cleaning device and its cleaning method |
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| CN110702490A (en) * | 2019-11-01 | 2020-01-17 | 上海申和热磁电子有限公司 | Method for purifying and analyzing silicon carbide in semiconductor slice waste liquid |
| CN110860223A (en) * | 2019-12-05 | 2020-03-06 | 南京工业大学东海先进硅基材料研究院 | Grading method of superfine silicon carbide micro powder with narrow particle size distribution |
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