CN104211064B - A kind of impurity removal process promoting fine powder of silicon carbide quality - Google Patents
A kind of impurity removal process promoting fine powder of silicon carbide quality Download PDFInfo
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- CN104211064B CN104211064B CN201410434542.XA CN201410434542A CN104211064B CN 104211064 B CN104211064 B CN 104211064B CN 201410434542 A CN201410434542 A CN 201410434542A CN 104211064 B CN104211064 B CN 104211064B
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Abstract
A kind of impurity removal process promoting fine powder of silicon carbide quality, relate to the impurity-removing method of silicon carbide micro-powder, first fine powder of silicon carbide is added deionized water and is configured to the slip that concentration is 30%, and add foaming agent and the polyoxyethylene of slip gross weight 0.01%, then slip is delivered to column flotation de-carbon, then the slip after flotation being processed is delivered to wet magnetic separator and is carried out iron removal by magnetic separation, repeat aforesaid operations, until the foam in flotation column becomes canescence from depth to shallow, then stop flotation and magnetic separation process, then by from wet magnetic separator out pulp density dilution, and add surfactant, it is then sent to cyclone classification system and removes the particle of less than 5.5 microns, again through dehydrate, i.e. can get Fe2O3≤ 0.4%, free carbon≤0.3%, the high-quality silicon carbide fine powder of sub-content≤3.5%.Silicon carbide micro-powder stay in grade, cleanliness factor prepared by the present invention are high, and production technology is simple, and the process time significantly shortens.
Description
Technical field
The present invention relates to a kind of impurity removal process method of fine powder of silicon carbide, be specifically related to before fine powder of silicon carbide classification fine powder of silicon carbide pretreatment, the impurity removal process that promotes physical and chemical index.
Background technology
Fine powder of silicon carbide product is as photovoltaic industry, the important auxiliary material of semicon industry crystalline silicon line cutting, and the physical and chemical index of its product has higher requirement.Free carbon contained in fine powder of silicon carbide raw material, iron sesquioxide, particulate fine powder are mainly controlled by promoting of its physical and chemical index the most targeted, after the process used mostly is addition foaming agent, manually foam is pulled out, reach to remove the purpose of free carbon, use bar magnet absorption irony, reach to remove the purpose of iron sesquioxide in raw material, use natural sedimentation to remove particulate fine powder.Said method treatment effect is unsatisfactory, efficiency is low, and it is bigger to put into artificial amount, through the material that said method processes, particulate fine powder content easily exceeds standard, and the product D94 of formation is low, does not reaches the requirement of product, and in the material after processing, the content of free carbon and iron sesquioxide is higher, affects the quality of fine powder of silicon carbide.
Summary of the invention
The technical problem to be solved is that in the fine powder of silicon carbide that existing fine powder of silicon carbide impurity removal process processes, particulate fine powder content easily exceeds standard and the content of free carbon and iron sesquioxide is higher, and the quality of fine powder of silicon carbide is unstable.
The technical scheme is that a kind of impurity removal process promoting fine powder of silicon carbide quality of the present invention, step is as follows:
(1), fine powder of silicon carbide is put in blending tank, add deionized water and be configured to the slip that mass concentration is 30%-50%, after stirring, deliver to slip have enough to meet the need in cylinder；
(2), the slip in turnover cylinder adds foaming agent and the polyoxyethylene of slip gross weight 0.01% of slip gross weight 0.01%；
(3), will deliver in flotation column added with foaming agent and polyoxyethylated slip, and bottom flotation column, be passed through air, and remove the foam produced in slurry level；
(4) slip, by flotation column processed is delivered to wet magnetic separator and is carried out magnetic separation, removes the Fe in slip2O3；
(5) in, the slip processed by wet magnetic separator delivers to described turnover cylinder again, add water and its concentration is adjusted to 30%-50%, it is subsequently adding foaming agent and the polyoxyethylene of slip gross weight 0.01% of the slip gross weight 0.01% after adjusting concentration, carries out flotation and magnetic separation according to the method for step (3) and step (4) successively；Repeat aforesaid operations, until the foam in flotation column becomes canescence from depth to shallow, then stop flotation and magnetic separation process, and particulate fine powder tank will be delivered to from wet magnetic separator slip out；
(6), adding deionized water in the slip delivering to particulate fine powder tank, the mass concentration of regulation slip is 10%-30%, and adds the surfactant of slip gross weight 0.5 ‰ in slip；
(7), by the slurry pipeline transport in particulate fine powder tank to cyclone, circular treatment 2-5 time, to remove the fine particles in slip, the internal diameter of cyclone is 10mm ~ 55mm, the feed pressure of slip is 0.1Mpa ~ 0.2Mpa, and the slip after process, through dehydrate, i.e. can get Fe2O3≤ 0.4%, free carbon≤0.3%, the high-quality silicon carbide fine powder of less than 5.5 microns particle content≤3.5%.
Described foaming agent is quaternary ammonium salt, sulfonyl hydrazines compound or dodecylbenzene sodium sulfonate.
Described surfactant is sodium lauryl sulphate, cellulose derivative, polyacrylamide or fatty acid polyethylene glycol ester.
The present invention is designed by system, reagent rational proportion, defines the most complete process controlling carborundum physical and chemical index, and its physical and chemical index that can be good at promoting fine powder of silicon carbide forms the fine powder of silicon carbide of high-quality.The process of the present invention is carried out before fine powder of silicon carbide classification, fine powder of silicon carbide after present invention process can control the content of particulate fine powder in follow-up classification process further, reach the lifting again of product cleanliness factor, enable the fine powder of silicon carbide product ultimately formed to reach high quality and cleanliness factor.
Beneficial effect: silicon carbide slurry is taked in present invention process mode alternately carry out de-carbon and except ferrum, simultaneously, de-carbon and iron removal is made to circulate operation continuously, so that the content of free carbon in the fine powder of silicon carbide finally given and iron sesquioxide is down to Fe2O3≤ 0.4%, free carbon≤0.3%, improve the cleanliness factor of fine powder of silicon carbide.Before flotation de-carbon, in addition to adding foaming agent in slip, it is also added into polyoxyethylene, is beneficial to improve the effect of flotation de-carbon.The present invention will complete de-carbon and processes except the silicon carbide slurry of ferrum delivers to cyclone classification system, in order to remove the particle (the i.e. described particulate fine powder in fine powder of silicon carbide) of in slip less than 5.5 microns, regulate the concentration of slip and in slip, add surfactant, the fine particles in slip can be made to be uniformly dispersed, it is more conducive to remove particulate fine powder, the method finally making particle content≤3.5% of less than 5.5 microns, relatively natural sedimentation in fine powder of silicon carbide is removed particulate fine powder effect and to be got well.The present invention can process the low grade carborundum fine powder of SiC≤98%, and carborundum fine powder stay in grade, cleanliness factor after process are high, and production technology is simple, and automaticity is high, and the process time is greatly shortened.
Detailed description of the invention
A kind of impurity removal process promoting fine powder of silicon carbide quality, step is as follows:
(1), fine powder of silicon carbide is put in blending tank, add deionized water and be configured to the slip that mass concentration is 30%-50%, after stirring, deliver to slip have enough to meet the need in cylinder；
(2), the slip in turnover cylinder adds foaming agent and the polyoxyethylene of slip gross weight 0.01% of slip gross weight 0.01%；
(3), will deliver in flotation column added with foaming agent and polyoxyethylated slip, and bottom flotation column, be passed through air, and remove the foam produced in slurry level；
(4) slip, by flotation column processed is delivered to wet magnetic separator and is carried out magnetic separation, removes the Fe in slip2O3；
(5) in, the slip processed by wet magnetic separator delivers to described turnover cylinder again, add water and its concentration is adjusted to 30%-50%, it is subsequently adding foaming agent and the polyoxyethylene of slip gross weight 0.01% of the slip gross weight 0.01% after adjusting concentration, carries out flotation and magnetic separation according to the method for step (3) and step (4) successively；Repeat aforesaid operations, until the foam in flotation column becomes canescence from depth to shallow, then stop flotation and magnetic separation process, and particulate fine powder tank will be delivered to from wet magnetic separator slip out；
(6), adding deionized water in the slip delivering to particulate fine powder tank, the mass concentration of regulation slip is 10%-30%, and adds the surfactant of slip gross weight 0.5 ‰ in slip；
(7), by the slurry pipeline transport in particulate fine powder tank to cyclone, circular treatment 2-5 time, to remove the fine particles in slip, the internal diameter of cyclone is 10mm ~ 55mm, the feed pressure of slip is 0.1Mpa ~ 0.2Mpa, and the slip after process, through dehydrate, i.e. can get Fe2O3≤ 0.4%, free carbon≤0.3%, the high-quality silicon carbide fine powder of less than 5.5 microns particle content≤3.5%.
Described foaming agent is quaternary ammonium salt, sulfonyl hydrazines compound or dodecylbenzene sodium sulfonate.
Described surfactant is sodium lauryl sulphate, cellulose derivative, polyacrylamide or fatty acid polyethylene glycol ester.
Embodiment 1
nullFine powder of silicon carbide is put in blending tank，Add deionized water and be configured to the slip that mass concentration is 30%，After stirring，Deliver to slip have enough to meet the need in cylinder，Turnover cylinder is connected by pipeline with flotation column，Slip in turnover cylinder adds quaternary ammonium salt foaming agent (such as dodecyl dimethyl benzyl ammonium chloride) and the polyoxyethylene of slip gross weight 0.01% of slip gross weight 0.01%，Then slip is delivered to flotation column and carries out flotation de-carbon，Air it is passed through bottom flotation column，And remove the foam produced in slurry level，The slip that flotation column discharging opening flows out is delivered to wet magnetic separator by pipeline and is carried out iron removal by magnetic separation，The slip that wet magnetic separator processed is delivered to have enough to meet the need in cylinder again，Add water and its concentration is adjusted to 30%，And add foaming agent and the polyoxyethylene of slip gross weight 0.01% of the slip gross weight 0.01% after adjusting concentration，Carry out flotation and magnetic separation process the most successively，Slip is at turnover cylinder、Circular treatment between flotation column and wet magnetic separator，Repeat aforesaid operations，Until the foam in flotation column becomes canescence from depth to shallow，Then stop flotation and magnetic separation process，And particulate fine powder tank will be delivered to from wet magnetic separator slip out，The mass concentration being subsequently adding deionized water regulation slip is 10%，And in slip, add the sodium lauryl sulphate of slip gross weight 0.5 ‰，Then by the slurry pipeline transport in particulate fine powder tank to the cyclone classification system being made up of multiple cyclones being arranged in parallel，The internal diameter of cyclone is 10mm ~ 55mm，The feed pressure of slip is 0.1Mpa，After circular treatment 2 times，Slip is through dehydrate，I.e. can get Fe2O3≤ 0.4%, free carbon≤0.3%, the high-quality silicon carbide fine powder of particle content≤3.5% of less than 5.5 microns.
Embodiment 2
nullFine powder of silicon carbide is put in blending tank，Add deionized water and be configured to the slip that mass concentration is 50%，After stirring，Deliver to slip have enough to meet the need in cylinder，Turnover cylinder is connected by pipeline with flotation column，Slip in turnover cylinder adds sulfohydrazide type blowing agent and the polyoxyethylene of slip gross weight 0.01% of slip gross weight 0.01%，Then slip is delivered to flotation column and carries out flotation de-carbon，Air it is passed through bottom flotation column，And remove the foam produced in slurry level，The slip that flotation column discharging opening flows out is delivered to wet magnetic separator by pipeline and is carried out iron removal by magnetic separation，The slip that wet magnetic separator processed is delivered to have enough to meet the need in cylinder again，Add water and its concentration is adjusted to 50%，And add foaming agent and the polyoxyethylene of slip gross weight 0.01% of the slip gross weight 0.01% after adjusting concentration，Carry out flotation and magnetic separation process the most successively，Slip is at turnover cylinder、Circular treatment between flotation column and wet magnetic separator，Repeat aforesaid operations，Until the foam in flotation column becomes canescence from depth to shallow，Then stop flotation and magnetic separation process，And particulate fine powder tank will be delivered to from wet magnetic separator slip out，The mass concentration being subsequently adding deionized water regulation slip is 30%，And in slip, add the polyacrylamide of slip gross weight 0.5 ‰，Then by the slurry pipeline transport in particulate fine powder tank to the cyclone classification system being made up of multiple cyclones being arranged in parallel，The internal diameter of cyclone is 10mm ~ 55mm，The feed pressure of slip is 0.1Mpa，After circular treatment 5 times，Slip is through dehydrate，I.e. can get Fe2O3≤ 0.4%, free carbon≤0.3%, the high-quality silicon carbide fine powder of particle content≤3.5% of less than 5.5 microns.
Embodiment 3
nullFine powder of silicon carbide is put in blending tank，Add deionized water and be configured to the slip that mass concentration is 40%，After stirring，Deliver to slip have enough to meet the need in cylinder，Turnover cylinder is connected by pipeline with flotation column，Slip in turnover cylinder adds dodecylbenzene sodium sulfonate and the polyoxyethylene of slip gross weight 0.01% of slip gross weight 0.01%，Then slip is delivered to flotation column and carries out flotation de-carbon，Air it is passed through bottom flotation column，And remove the foam produced in slurry level，The slip that flotation column discharging opening flows out is delivered to wet magnetic separator by pipeline and is carried out iron removal by magnetic separation，The slip that wet magnetic separator processed is delivered to have enough to meet the need in cylinder again，Add water and its concentration is adjusted to 40%，And add foaming agent and the polyoxyethylene of slip gross weight 0.01% of the slip gross weight 0.01% after adjusting concentration，Carry out flotation and magnetic separation process the most successively，Slip is at turnover cylinder、Circular treatment between flotation column and wet magnetic separator，Repeat aforesaid operations，Until the foam in flotation column becomes canescence from depth to shallow，Then stop flotation and magnetic separation process，And particulate fine powder tank will be delivered to from wet magnetic separator slip out，The mass concentration being subsequently adding deionized water regulation slip is 20%，And in slip, add the fatty acid polyethylene glycol ester of slip gross weight 0.5 ‰，Then by the slurry pipeline transport in particulate fine powder tank to the cyclone classification system being made up of multiple cyclones being arranged in parallel，The internal diameter of cyclone is 10mm ~ 55mm，The feed pressure of slip is 0.2Mpa，After circular treatment 3 times，Slip is through dehydrate，I.e. can get Fe2O3≤ 0.4%, free carbon≤0.3%, the high-quality silicon carbide fine powder of particle content≤3.5% of less than 5.5 microns.
Claims (1)
1. the impurity removal process promoting fine powder of silicon carbide quality, it is characterised in that: step is as follows:
(1), fine powder of silicon carbide is put in blending tank, add deionized water and be configured to the slip that mass concentration is 30%-50%, after stirring, deliver to slip have enough to meet the need in cylinder；
(2), the slip in turnover cylinder adds foaming agent and the polyoxyethylene of slip gross weight 0.01% of slip gross weight 0.01%；
(3), will deliver in flotation column added with foaming agent and polyoxyethylated slip, and bottom flotation column, be passed through air, and remove the foam produced in slurry level；Described foaming agent is quaternary ammonium salt, sulfonyl hydrazines compound or dodecylbenzene sodium sulfonate；
(4) slip, by flotation column processed is delivered to wet magnetic separator and is carried out magnetic separation, removes the Fe in slip2O3；
(5) in, the slip processed by wet magnetic separator delivers to described turnover cylinder again, add water and its concentration is adjusted to 30%-50%, it is subsequently adding foaming agent and the polyoxyethylene of slip gross weight 0.01% of the slip gross weight 0.01% after adjusting concentration, carries out flotation and magnetic separation according to the method for step (3) and step (4) successively；Repeat aforesaid operations, until the foam in flotation column becomes canescence from depth to shallow, then stop flotation and magnetic separation process, and particulate fine powder tank will be delivered to from wet magnetic separator slip out；
(6), adding deionized water in the slip delivering to particulate fine powder tank, the mass concentration of regulation slip is 10%-30%, and adds the surfactant of slip gross weight 0.5 ‰ in slip；Described surfactant is sodium lauryl sulphate, cellulose derivative, polyacrylamide or fatty acid polyethylene glycol ester；
(7), by the slurry pipeline transport in particulate fine powder tank to cyclone, circular treatment 2-5 time, to remove the fine particles in slip, the internal diameter of cyclone is 10mm ~ 55mm, the feed pressure of slip is 0.1Mpa ~ 0.2Mpa, and the slip after process, through dehydrate, i.e. can get Fe2O3≤ 0.4%, free carbon≤0.3%, the high-quality silicon carbide fine powder of less than 5.5 microns particle content≤3.5%.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN105600787B (en) * | 2016-03-21 | 2017-09-01 | 平顶山市国邦新材料有限公司 | A kind of carborundum impurity removed 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 |
| CN105621415B (en) * | 2016-03-21 | 2017-11-07 | 平顶山市国邦新材料有限公司 | A kind of silicon carbide slurry settles homogenization system |
| CN106365168A (en) * | 2016-08-31 | 2017-02-01 | 平顶山易成新材料有限公司 | Method for purifying carbon materials in silicon carbide |
| CN111960419A (en) * | 2020-08-27 | 2020-11-20 | 惠州市中惠宇航半导体新材料有限公司 | Silicon carbide superfine powder and production method thereof |
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| US6569397B1 (en) * | 2000-02-15 | 2003-05-27 | Tapesh Yadav | Very high purity fine powders and methods to produce such powders |
| CN101130237A (en) * | 2007-09-11 | 2008-02-27 | 西安交通大学 | Method for recycling silica powder and carborundum powder from cut waste mortar |
| CN102285654A (en) * | 2011-06-02 | 2011-12-21 | 江苏大阳光辅股份有限公司 | Production method of silicon wafer cutting blade material |
| CN102951641A (en) * | 2012-11-01 | 2013-03-06 | 临沭山田研磨材有限公司 | Water-saving and environmental protection-type preparation method of silicon carbide micro-powder for silicon wafer wire cutting |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6569397B1 (en) * | 2000-02-15 | 2003-05-27 | Tapesh Yadav | Very high purity fine powders and methods to produce such powders |
| CN101130237A (en) * | 2007-09-11 | 2008-02-27 | 西安交通大学 | Method for recycling silica powder and carborundum powder from cut waste mortar |
| CN102285654A (en) * | 2011-06-02 | 2011-12-21 | 江苏大阳光辅股份有限公司 | Production method of silicon wafer cutting blade material |
| CN102951641A (en) * | 2012-11-01 | 2013-03-06 | 临沭山田研磨材有限公司 | Water-saving and environmental protection-type preparation method of silicon carbide micro-powder for silicon wafer wire cutting |
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