CN104211064A - Impurity removing process for enhancing quality of silicon carbide fine micro powder - Google Patents
Impurity removing process for enhancing quality of silicon carbide fine micro powder Download PDFInfo
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- CN104211064A CN104211064A CN201410434542.XA CN201410434542A CN104211064A CN 104211064 A CN104211064 A CN 104211064A CN 201410434542 A CN201410434542 A CN 201410434542A CN 104211064 A CN104211064 A CN 104211064A
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- slip
- silicon carbide
- fine powder
- flotation
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Abstract
The invention discloses an impurity removing process for enhancing quality of silicon carbide fine micro powder and relates to an impurity removing method of silicon carbide micro powder. The process comprises the following steps: firstly, adding the silicon carbide fine micro powder into deionized water to prepare 30% slurry, and adding a foaming agent and polyoxyethylene which account for 0.01% of the total weight of the slurry; then, feeding the slurry to a flotation column to float and decarbonize; then, feeding the floated slurry to a wet magnetic separator for magnetic separation to remove iron; repeating the above operations till foam in the floatation column changes from being deep to being light and is off-white and stopping flotation and magnetic separation process; then, diluting the concentration of the slurry discharged from the wet magnetic separator, and adding a surfactant; then, feeding to a cyclone grading system to remove particles which are less than 5.5 microns; and then dehydrating and drying to obtain high quality silicon carbide fine micro powder with Fe2O3 less than or equal to 0.4%, free carbon less than or equal to 0.3% and particle content less than or equal to 3.5%. The silicon carbide fine micro powder disclosed by the invention is stable in quality, high in cleanliness and simple in production process, and the treatment time is greatly shortened.
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 the front impurity removal process to fine powder of silicon carbide pre-treatment, lifting physical and chemical index of fine powder of silicon carbide classification.
Background technology
Fine powder of silicon carbide product is as the important auxiliary material of photovoltaic industry, semicon industry crystalline silicon Linear cut, and the physical and chemical index of its product has higher requirement.Current the lifting for its physical and chemical index mainly controls uncombined carbon contained in fine powder of silicon carbide raw material, ferric oxide, particulate fine powder, after the processing method adopted mostly is and adds whipping agent, manually foam is pulled out, reach the object removing uncombined carbon, adopt bar magnet absorption irony, reach the object removing ferric oxide in raw material, adopt natural sedimentation to remove particulate fine powder.Aforesaid method treatment effect is unsatisfactory, efficiency is low, and the manually amount that drops into is larger, through the material of aforesaid method process, particulate fine powder content easily exceeds standard, and the product D94 of formation is low, does not reach the requirement of product, and material Free Carbon after process and the content of ferric oxide higher, affect the quality of fine powder of silicon carbide.
Summary of the invention
Technical problem to be solved by this invention is that in the fine powder of silicon carbide of existing fine powder of silicon carbide impurity removal process process, particulate fine powder content easily exceeds standard and the content of uncombined carbon and ferric oxide is higher, and the quality of fine powder of silicon carbide is unstable.
The technical scheme that the present invention is adopted for achieving the above object is: a kind of impurity removal process promoting fine powder of silicon carbide quality, and step is as follows:
(1), by fine powder of silicon carbide drop in mixing tank, add deionized water and be mixed with the slip that mass concentration is 30%-50%, after stirring, slip is delivered in turnover cylinder;
(2), in the slip in turnover cylinder, the whipping agent of slip gross weight 0.01% and the polyoxyethylene of slip gross weight 0.01% is added;
(3), whipping agent will be added with and polyoxyethylated slip is delivered in flotation column, and bottom flotation column, pass into air, and remove the foam that slurry level produces;
(4), by the slip of flotation column process deliver to wet magnetic separator and carry out magnetic separation, the Fe in removing slip
2o
3;
(5), the slip of wet magnetic separator process is delivered to again in described turnover cylinder, add water and its concentration is adjusted to 30%-50%, then add the whipping agent of slip gross weight 0.01% after adjustment concentration and the polyoxyethylene of slip gross weight 0.01%, carry 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 deliver to particulate fine powder tank by from wet magnetic separator slip out;
(6), in the slip delivering to particulate fine powder tank add deionized water, the mass concentration regulating slip is 10%-30%, and in slip, add the tensio-active agent of slip gross weight 0.5 ‰;
(7), by the slurry pipeline transport in particulate fine powder tank to swirler, circular treatment 2-5 time, to remove the fine particles in slip, the internal diameter of swirler is 10mm ~ 55mm, the feed pressure of slip is 0.1Mpa ~ 0.2Mpa, and the slip after process, through dehydrating, can obtain Fe
2o
3≤ 0.4%, uncombined carbon≤0.3%, the high-quality silicon carbide fine powder of less than 5.5 microns particle content≤3.5%.
Described whipping agent is quaternary ammonium salt, sulfonyl hydrazines compound or Sodium dodecylbenzene sulfonate.
Described tensio-active agent is sodium lauryl sulphate, derivatived cellulose, polyacrylamide or fatty acid polyglycol ester.
The present invention is by system design, and reagent rational proportion, defines the processing method of comparatively complete control silicon carbide physical and chemical index, and it can be good at the physical and chemical index promoting fine powder of silicon carbide, forms the fine powder of silicon carbide of high-quality.Processing method of the present invention is carried out before fine powder of silicon carbide classification, fine powder of silicon carbide after process of the present invention can control the content of particulate fine powder further in follow-up classification process, reach the lifting again of product cleanliness factor, enable the final fine powder of silicon carbide product formed reach high quality and cleanliness factor.
Beneficial effect: take the mode hocketed to come de-carbon and deironing to silicon carbide slurry in present invention process, simultaneously, make de-carbon and the operation of iron removal continuous circulation, thus make the content of the uncombined carbon in the fine powder of silicon carbide finally obtained and ferric oxide be down to Fe
2o
3≤ 0.4%, uncombined carbon≤0.3%, improves the cleanliness factor of fine powder of silicon carbide.Before flotation de-carbon, add except whipping agent except in slip, also add polyoxyethylene, be beneficial to the effect improving flotation de-carbon.The silicon carbide slurry completing de-carbon and deironing is delivered to cyclone classification system and is processed by the present invention, in order to remove the particle (the particulate fine powder in namely described fine powder of silicon carbide) of in slip less than 5.5 microns, regulate the concentration of slip and add tensio-active agent in slip, the fine particles in slip can be made to be uniformly dispersed, be more conducive to remove particulate fine powder, finally make particle content≤3.5% of in fine powder of silicon carbide less than 5.5 microns, removing particulate fine powder effect compared with the method for natural sedimentation will get well.The present invention can the low grade silicon carbide fine powder of processing of SiC≤98%, and the silicon carbide fine powder stay in grade after process, cleanliness factor are high, and production technique is simple, and level of automation is high, and the treatment time significantly shortens.
Embodiment
Promote an impurity removal process for fine powder of silicon carbide quality, step is as follows:
(1), by fine powder of silicon carbide drop in mixing tank, add deionized water and be mixed with the slip that mass concentration is 30%-50%, after stirring, slip is delivered in turnover cylinder;
(2), in the slip in turnover cylinder, the whipping agent of slip gross weight 0.01% and the polyoxyethylene of slip gross weight 0.01% is added;
(3), whipping agent will be added with and polyoxyethylated slip is delivered in flotation column, and bottom flotation column, pass into air, and remove the foam that slurry level produces;
(4), by the slip of flotation column process deliver to wet magnetic separator and carry out magnetic separation, the Fe in removing slip
2o
3;
(5), the slip of wet magnetic separator process is delivered to again in described turnover cylinder, add water and its concentration is adjusted to 30%-50%, then add the whipping agent of slip gross weight 0.01% after adjustment concentration and the polyoxyethylene of slip gross weight 0.01%, carry 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 deliver to particulate fine powder tank by from wet magnetic separator slip out;
(6), in the slip delivering to particulate fine powder tank add deionized water, the mass concentration regulating slip is 10%-30%, and in slip, add the tensio-active agent of slip gross weight 0.5 ‰;
(7), by the slurry pipeline transport in particulate fine powder tank to swirler, circular treatment 2-5 time, to remove the fine particles in slip, the internal diameter of swirler is 10mm ~ 55mm, the feed pressure of slip is 0.1Mpa ~ 0.2Mpa, and the slip after process, through dehydrating, can obtain Fe
2o
3≤ 0.4%, uncombined carbon≤0.3%, the high-quality silicon carbide fine powder of less than 5.5 microns particle content≤3.5%.
Described whipping agent is quaternary ammonium salt, sulfonyl hydrazines compound or Sodium dodecylbenzene sulfonate.
Described tensio-active agent is sodium lauryl sulphate, derivatived cellulose, polyacrylamide or fatty acid polyglycol ester.
Embodiment 1
Fine powder of silicon carbide is dropped in mixing tank, add deionized water and be mixed with the slip that mass concentration is 30%, after stirring, slip is delivered in turnover cylinder, turnover cylinder is connected by pipeline with flotation column, the quaternary ammonium salt whipping agent (as dodecyl benzyl dimethyl ammonium chloride) of slip gross weight 0.01% and the polyoxyethylene of slip gross weight 0.01% is added in the slip in turnover cylinder, then slip is delivered to flotation column and carry out flotation de-carbon, air is passed into bottom flotation column, and remove the foam that slurry level produces, the slip that flotation column discharge port flows out is delivered to wet magnetic separator by pipeline and is carried out iron removal by magnetic separation, the slip of wet magnetic separator process is delivered in turnover cylinder again, add water and its concentration is adjusted to 30%, and the whipping agent of slip gross weight 0.01% added after adjustment concentration and the polyoxyethylene of slip gross weight 0.01%, and then carry out flotation and magnetic separation process 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 deliver to particulate fine powder tank by from wet magnetic separator slip out, then adding deionized water regulates the mass concentration of slip to be 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 that is made up of multiple swirler be arranged in parallel, the internal diameter of swirler is 10mm ~ 55mm, the feed pressure of slip is 0.1Mpa, after circular treatment 2 times, slip is through dehydrating, Fe can be obtained
2o
3≤ 0.4%, uncombined carbon≤0.3%, the high-quality silicon carbide fine powder of particle content≤3.5% of less than 5.5 microns.
Embodiment 2
Fine powder of silicon carbide is dropped in mixing tank, add deionized water and be mixed with the slip that mass concentration is 50%, after stirring, slip is delivered in turnover cylinder, turnover cylinder is connected by pipeline with flotation column, the sulfohydrazide type blowing agent of slip gross weight 0.01% and the polyoxyethylene of slip gross weight 0.01% is added in the slip in turnover cylinder, then slip is delivered to flotation column and carry out flotation de-carbon, air is passed into bottom flotation column, and remove the foam that slurry level produces, the slip that flotation column discharge port flows out is delivered to wet magnetic separator by pipeline and is carried out iron removal by magnetic separation, the slip of wet magnetic separator process is delivered in turnover cylinder again, add water and its concentration is adjusted to 50%, and the whipping agent of slip gross weight 0.01% added after adjustment concentration and the polyoxyethylene of slip gross weight 0.01%, and then carry out flotation and magnetic separation process 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 deliver to particulate fine powder tank by from wet magnetic separator slip out, then adding deionized water regulates the mass concentration of slip to be 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 that is made up of multiple swirler be arranged in parallel, the internal diameter of swirler is 10mm ~ 55mm, the feed pressure of slip is 0.1Mpa, after circular treatment 5 times, slip is through dehydrating, Fe can be obtained
2o
3≤ 0.4%, uncombined carbon≤0.3%, the high-quality silicon carbide fine powder of particle content≤3.5% of less than 5.5 microns.
Embodiment 3
Fine powder of silicon carbide is dropped in mixing tank, add deionized water and be mixed with the slip that mass concentration is 40%, after stirring, slip is delivered in turnover cylinder, turnover cylinder is connected by pipeline with flotation column, the Sodium dodecylbenzene sulfonate of slip gross weight 0.01% and the polyoxyethylene of slip gross weight 0.01% is added in the slip in turnover cylinder, then slip is delivered to flotation column and carry out flotation de-carbon, air is passed into bottom flotation column, and remove the foam that slurry level produces, the slip that flotation column discharge port flows out is delivered to wet magnetic separator by pipeline and is carried out iron removal by magnetic separation, the slip of wet magnetic separator process is delivered in turnover cylinder again, add water and its concentration is adjusted to 40%, and the whipping agent of slip gross weight 0.01% added after adjustment concentration and the polyoxyethylene of slip gross weight 0.01%, and then carry out flotation and magnetic separation process 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 deliver to particulate fine powder tank by from wet magnetic separator slip out, then adding deionized water regulates the mass concentration of slip to be 20%, and in slip, add the fatty acid polyglycol ester of slip gross weight 0.5 ‰, then by the slurry pipeline transport in particulate fine powder tank to the cyclone classification system that is made up of multiple swirler be arranged in parallel, the internal diameter of swirler is 10mm ~ 55mm, the feed pressure of slip is 0.2Mpa, after circular treatment 3 times, slip is through dehydrating, Fe can be obtained
2o
3≤ 0.4%, uncombined carbon≤0.3%, the high-quality silicon carbide fine powder of particle content≤3.5% of less than 5.5 microns.
Claims (3)
1. promote an impurity removal process for fine powder of silicon carbide quality, it is characterized in that: step is as follows:
(1), by fine powder of silicon carbide drop in mixing tank, add deionized water and be mixed with the slip that mass concentration is 30%-50%, after stirring, slip is delivered in turnover cylinder;
(2), in the slip in turnover cylinder, the whipping agent of slip gross weight 0.01% and the polyoxyethylene of slip gross weight 0.01% is added;
(3), whipping agent will be added with and polyoxyethylated slip is delivered in flotation column, and bottom flotation column, pass into air, and remove the foam that slurry level produces;
(4), by the slip of flotation column process deliver to wet magnetic separator and carry out magnetic separation, the Fe in removing slip
2o
3;
(5), the slip of wet magnetic separator process is delivered to again in described turnover cylinder, add water and its concentration is adjusted to 30%-50%, then add the whipping agent of slip gross weight 0.01% after adjustment concentration and the polyoxyethylene of slip gross weight 0.01%, carry 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 deliver to particulate fine powder tank by from wet magnetic separator slip out;
(6), in the slip delivering to particulate fine powder tank add deionized water, the mass concentration regulating slip is 10%-30%, and in slip, add the tensio-active agent of slip gross weight 0.5 ‰;
(7), by the slurry pipeline transport in particulate fine powder tank to swirler, circular treatment 2-5 time, to remove the fine particles in slip, the internal diameter of swirler is 10mm ~ 55mm, the feed pressure of slip is 0.1Mpa ~ 0.2Mpa, and the slip after process, through dehydrating, can obtain Fe
2o
3≤ 0.4%, uncombined carbon≤0.3%, the high-quality silicon carbide fine powder of less than 5.5 microns particle content≤3.5%.
2. a kind of impurity removal process promoting fine powder of silicon carbide quality as claimed in claim 1, is characterized in that: described whipping agent is quaternary ammonium salt, sulfonyl hydrazines compound or Sodium dodecylbenzene sulfonate.
3. a kind of impurity removal process promoting fine powder of silicon carbide quality as claimed in claim 1, is characterized in that: described tensio-active agent is sodium lauryl sulphate, derivatived cellulose, polyacrylamide or fatty acid polyglycol ester.
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| CN201410434542.XA CN104211064B (en) | 2014-08-29 | 2014-08-29 | A kind of impurity removal process promoting fine powder of silicon carbide quality |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105127009A (en) * | 2015-08-26 | 2015-12-09 | 连云港龙塔研磨材料有限公司 | Flotation device and method for removing free carbon in silicon carbide powder |
| 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 |
| CN105600787A (en) * | 2016-03-21 | 2016-05-25 | 平顶山市国邦新材料有限公司 | Silicon carbide impurity removal system |
| CN105621415A (en) * | 2016-03-21 | 2016-06-01 | 平顶山市国邦新材料有限公司 | Silicon carbide slurry sedimentation 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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| 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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| 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 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105127009A (en) * | 2015-08-26 | 2015-12-09 | 连云港龙塔研磨材料有限公司 | Flotation device and method for removing free carbon in silicon carbide powder |
| 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 |
| CN105600787A (en) * | 2016-03-21 | 2016-05-25 | 平顶山市国邦新材料有限公司 | Silicon carbide impurity removal system |
| CN105621415A (en) * | 2016-03-21 | 2016-06-01 | 平顶山市国邦新材料有限公司 | Silicon carbide slurry sedimentation homogenization 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 |
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| 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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