CN102285653B - Method for removing carbon impurities in silicon carbide micropowder - Google Patents
Method for removing carbon impurities in silicon carbide micropowder Download PDFInfo
- Publication number
- CN102285653B CN102285653B CN2011101464423A CN201110146442A CN102285653B CN 102285653 B CN102285653 B CN 102285653B CN 2011101464423 A CN2011101464423 A CN 2011101464423A CN 201110146442 A CN201110146442 A CN 201110146442A CN 102285653 B CN102285653 B CN 102285653B
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- slurry
- removing carbon
- carbon impurities
- micropowder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention discloses a method for removing carbon impurities in silicon carbide micropowder. The method comprises the following steps: injecting water into silicon carbide micropowder to prepare slurry, adding a dispersant in the slurry to adjust the PH value, centrifuging the silicon carbide slurry by a centrifugal device, injecting water into the slurry again to prepare slurry, adding floatation oil in the slurry, injecting the mixture into a hydraulic classification device, continuously pumping air to stir, performing hydraulic flotation, then performing alkali washing to the obtained slurry, adjusting the PH value, cleaning, adding a filter aid, performing pressure filtration, placing the product in the oxidizing atmosphere to perform forced drying, and then cooling to room temperature to obtain the purified silicon carbide micropowder product. By adopting the method, the circulation of industrial water can be realized; and silicon carbide is dried in the oxidizing atmosphere, the stability and reliability of the silicon carbide micropowder can be increased, the flow is simple, the equipment dependency degree is low, and the method is suitable for industrialized mass production.
Description
Technical field
The present invention relates to the purification of silicon-containing compound, be specifically related to a kind of method of removing carbon impurities in silicon carbide micropowder.
Background technology
Continuous exploitation and the use of the non-regeneration energies such as coal oil will be at the many decades internal consumption totally.R and D to new sustainable development source have obtained paying close attention to widely.Under this background, the silicon solar photovoltaic technology has obtained flourish.High-quality silicon wafer is the parts of most critical in the photovoltaic conversion, and in the processing of present silicon wafer, and the sheet material that the linear cutting equipment by special use cuts into different diameter and thickness with silicon rod or silicon ingot is present general mode in the world.This incision principle is to be that the steel wire of 120～160 μ is cut vector with thousands of diameters, the employing wettability is good, chip removal ability is strong, the cutting fluids such as the polyethylene glycols of good dispersity, propandiols make the silicon carbide blade material Uniform Dispersion of high rigidity as main slurry, as the main cutting medium, by the rapid movement of steel wire on the silicon ingot surface, drive slurry in the silicon ingot surface flow, make silicon carbide blade material and silicon ingot that cutting and friction occur, silicon ingot cuts into the smooth isometrical sheet material of multi-disc smooth surface the most at last.
This shows, the quality of processing silicon wafer depends on the cutting quality of silicon carbide blade material.And to guarantee cutting quality, silicon carbide blade material should at first guarantee certain purity.But it is mostly standby by Acheson's legal system to process at present the employed raw material of silicon carbide blade material, namely uses at high temperature direct reaction synthesizing silicon carbide of graphite and quartz raw material, causes inevitably introducing carbon impurity.Therefore, the simple carbon impurity of removing efficiently becomes silicon carbide blade material processing industry problem anxious to be resolved.
Summary of the invention
The object of the invention is to overcome the defective that exists in the prior art, design a kind of simple efficiently method of removing carbon impurities in silicon carbide micropowder.
For achieving the above object, technical scheme of the present invention provides a kind of method of removing carbon impurities in silicon carbide micropowder, and the method for de-carbon impurity may further comprise the steps:
The first step: being filled to the stock quality percentage concentration in the ball milling silicon carbide micro-powder is 15%～30%, adds dispersion agent, adds acid and regulate pH value to 6.0～7.0 under the stirring of forced mixer;
Second step: adopt centrifugation apparatus that silicon carbide slurry is carried out centrifugal, reduce to below 20% to silicon carbide micro-powder moisture content;
The 3rd step: it is 25%～40% that the slurry that the upper step was obtained is filled to the stock quality percentage concentration again;
The 4th step: above-mentioned slurry is injected hydraulic grading device, add flotation oil, continue to blast pneumatic blending, then in hydraulic grading device, pass into current, utilize overflow to carry out hydraulic flotation;
The 5th step: the slurry behind hydraulic flotation is carried out alkali cleaning, adjust pH value to 7.5～8.5, clean, add flocculating aids, utilize the Filter Press slurry, gained slurry moisture content reduces to below 10%;
The 6th step: the slurry that obtained in the upper step inserted in the oxidizing atmosphere forces oven dry, after be cooled to room temperature, the silicon carbide micro-powder goods that obtain purifying.
Wherein, dispersion agent is Sudan Gum-arabic in the first step, Xylo-Mucine, six segregation sodium phosphates, at least a in the calcium sulfate; Dispersant dosage is slurry 80～220g per ton.
Wherein, acid is acetic acid in the first step, oxalic acid, at least a in 5%～20% the hydrochloric acid.
Wherein, flotation oil is pine camphor oil in the 4th step, oleic acid, and at least a in the QX-3 flotation oil, the consumption of flotation oil is slurry 100～160ml per ton.
Wherein, blasting air capacity in the 4th step is 1600～2300L/h.
Wherein, the hydraulic flotation flow velocity is 1200# silicon carbide micro-powder 420～880L/h in the 4th step, 1500# silicon carbide micro-powder 180～650L/h.
Wherein, the alkali cleaning medicine is lime in the 5th step, yellow soda ash, at least a in the water glass.
Wherein, flocculating aids is diatomite in the 5th step, perlite, medical stone, at least a in the atlapulgite; Drainage dosage is 4%～12% of stock quality; The granularity of flocculating aids is 50～150 orders.
Wherein, the oxygen level of the oxidizing atmosphere in the 6th step is greater than 40%; The drying temperature of described pressure oven dry is 180～220 ℃, and described slurry is dried to water content and is not more than 0.05%.
Wherein, centrifugation apparatus is horizontal spiral centrifuge or settling centrifuge in the second step; Pressure filter is plate and frame(type)filter press in described the 5th step; Forcing the equipment of oven dry in the 6th step is microwave dryer.
Advantage of the present invention and beneficial effect are: because simple flow of the present invention, the equipment dependency degree is low, and simple flow is fit to large-scale industrialization production, the silicon carbide micro-powder purity 99.9wt% behind the removal impurity; All kinds of flotation agent of the present invention and adjusting agent consumption are little, and little on the quality product impact, the environmental pollution impact is little.The water that flotation is used in the water can recycle, and has reduced Financial cost and has been conducive to environment protection; The present invention is dried silicon carbide micro-powder with oxidizing atmosphere, can oxidation removal residual minim carbon impurity and residual organic additive, and form the low-level oxidation layer on the silicon-carbide particle surface, remove the too sharp keen part in silicon-carbide particle surface, make the sword material when just bringing into use, be unlikely to cutting power and cause too by force quality fluctuation, improve stability in use and the reliability of silicon carbide blade material, thereby improved the cutting quality of silicon wafer.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples only are used for technical scheme of the present invention more clearly is described, and can not limit protection scope of the present invention with this.
Embodiment 1
The present invention is a kind of method of removing carbon impurities in silicon carbide micropowder, and the method for de-carbon impurity may further comprise the steps:
The first step: with the silicon carbide micro-powder water filling pulping of 1200#, the 400kg micro mist adds 1m
3Water, stock quality percentage concentration are 28.5wt%, add dispersion agent Xylo-Mucine 300g, and adding acetic acid adjustment pH value is 6, utilizes forced mixer fully to stir;
Second step: adopt horizontal spiral centrifuge, centrifugal rotational speed is 800r/min, and centrifugation time 3min reduces to below 20% moisture content;
The 3rd step: with the again water filling pulping of slurry that obtained in the upper step, the elementary slurry of 400kg adds 1.2m
3Water, stock quality percentage concentration are 25wt%
The 4th step: above-mentioned slurry injects hydraulic grading device, adds flotation oil pine camphor oil 160ml, continues to blast air 1600L/h and fully stirs, make flotation oil produce foam, pass into again the current that flow velocity is 560L/h, more than the lasting 2h, carbon impurity is fully flowed away with overflow, reach the removal of impurities purpose;
The 5th step: add yellow soda ash in the slurry that obtained in the upper step, adjusting pH value is 8.0, adds the diatomite of 7wt%, utilizes the plate and frame(type)filter press filter liquide, and moisture content is reduced to below 10%;
The 6th step: the slurry that obtained in the upper step is inserted in the general drying duct, and with oxygen level 45%, 210 ℃ of lower oven dry silicon-carbide particles of temperature obtain product.
Embodiment 2
The present invention is a kind of method of removing carbon impurities in silicon carbide micropowder, and the method for de-carbon impurity may further comprise the steps:
The first step: with the silicon carbide micro-powder water filling pulping of 1200#, the 400kg micro mist adds 2m
3Water, stock quality percentage concentration are 16.67wt%, add dispersion agent six segregation sodium phosphate 480g, and adding oxalic acid adjustment pH value is 6.5, utilizes forced mixer fully to stir;
Second step: adopt settling centrifuge, centrifugal rotational speed is 800r/min, and centrifugation time 3min reduces to below 20% moisture content;
The 3rd step: with the again water filling pulping of slurry that obtained in the upper step, the elementary slurry of 400kg adds 0.6m
3Water, stock quality percentage concentration are 40wt%;
The 4th step: above-mentioned slurry injects hydraulic grading device, adds flotation oil oleic acid 100ml, continues to blast air 2300L/h and fully stirs, make flotation oil produce foam, pass into again the current that flow velocity is 880L/h, more than the lasting 2h, carbon impurity is fully flowed away with overflow, reach the removal of impurities purpose;
The 5th step: add yellow soda ash in the slurry that obtained in the upper step, adjusting pH value is 7.5, adds the diatomite of 7wt%, utilizes the plate and frame(type)filter press filter liquide, and moisture content is reduced to below 10%;
The 6th step: the slurry that obtained in the upper step is inserted in the general drying duct, and with oxygen level 50%, 180 ℃ of lower oven dry silicon-carbide particles of temperature obtain product.
Embodiment 3
The present invention is a kind of method of removing carbon impurities in silicon carbide micropowder, and the method for de-carbon impurity may further comprise the steps:
The first step: with the silicon carbide micro-powder water filling pulping of 1500#, the 400kg micro mist adds 2m
3Water, stock quality percentage concentration are 16.67wt%, add dispersion agent Sudan Gum-arabic 250g, and adding acetic acid adjustment pH value is 6.5, utilizes forced mixer fully to stir;
Second step: adopt horizontal centrifuge, centrifugal rotational speed is 800r/min, and centrifugation time 3min reduces to below 20% moisture content;
The 3rd step: with the again water filling pulping of slurry that obtained in the upper step, the elementary slurry of 400kg adds 1.2m
3Water, stock quality percentage concentration are 25wt%;
The 4th step: above-mentioned slurry injects hydraulic grading device, adds flotation oil pine camphor oil 240ml, continues to blast air 2300L/h and fully stirs, make flotation oil produce foam, pass into again the current that flow velocity is 560L/h, more than the lasting 2h, carbon impurity is fully flowed away with overflow, reach the removal of impurities purpose;
The 5th step: add yellow soda ash in the slurry that obtained in the upper step, adjusting pH value is 8.0, adds the diatomite of 7wt%, utilizes the plate and frame(type)filter press filter liquide, and moisture content is reduced to below 10%;
The 6th step: the slurry that obtained in the upper step is inserted in the general drying duct, and with oxygen level 50%, 190 ℃ of lower oven dry silicon-carbide particles of temperature obtain product.
Embodiment 4
The present invention is a kind of method of removing carbon impurities in silicon carbide micropowder, and the method for de-carbon impurity may further comprise the steps:
The first step: with the silicon carbide micro-powder water filling pulping of 1500#, the 400kg micro mist adds 0.933m
3Water, stock quality percentage concentration are 30wt%, add dispersion agent calcium sulfate 300g, and adding acetic acid adjustment pH value is 7, utilizes forced mixer fully to stir;
Second step: adopt horizontal centrifuge, centrifugal rotational speed is 800r/min, and centrifugation time 3min reduces to below 20% moisture content;
The 3rd step: with the again water filling pulping of slurry that obtained in the upper step, the elementary slurry of 400kg adds 0.933m
3Water, stock quality percentage concentration are 30wt%;
The 4th step: above-mentioned slurry injects hydraulic grading device, adds QX-3 flotation oil 240ml, continues to blast air 1950L/h and fully stirs, make flotation oil produce foam, pass into again the current that flow velocity is 560L/h, more than the lasting 2h, carbon impurity is fully flowed away with overflow, reach the removal of impurities purpose;
The 5th step: add yellow soda ash in the slurry that obtained in the upper step, adjusting pH value is 8.5, adds the diatomite of 7wt%, utilizes the plate and frame(type)filter press filter liquide, and moisture content is reduced to below 10%;
The 6th step: the slurry that obtained in the upper step is inserted in the general drying duct, and with oxygen level 55%, 200 ℃ of lower oven dry silicon-carbide particles of temperature obtain product.
By above-mentioned art breading, gained silicon carbide micro-powder purity is up to 99.9%.
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. the method for a removing carbon impurities in silicon carbide micropowder is characterized in that, described de-carbon method may further comprise the steps:
The first step: being filled to the stock quality percentage concentration in the ball milling silicon carbide micro-powder is 15%～30%, adds dispersion agent, adds acid for adjusting pH value to 6.0～7.0 under the stirring of forced mixer;
Second step: adopt centrifugation apparatus that silicon carbide slurry is carried out centrifugal, reduce to below 20% to silicon carbide micro-powder moisture content;
The 3rd step: it is 25%～40% that the slurry that the upper step was obtained is filled to the stock quality percentage concentration again;
The 4th step: above-mentioned slurry is injected hydraulic grading device, add flotation oil, continue to blast pneumatic blending, then in hydraulic grading device, pass into current, utilize overflow to carry out hydraulic flotation;
The 5th step: the slurry behind hydraulic flotation is carried out alkali cleaning, adjust pH value to 7.5～8.5, clean, add flocculating aids, utilize the Filter Press slurry, gained slurry moisture content reduces to below 10%;
The 6th step: the slurry that obtained in the upper step inserted in the oxidizing atmosphere forces oven dry, after be cooled to room temperature, the silicon carbide micro-powder goods that obtain purifying.
2. the method for removing carbon impurities in silicon carbide micropowder as claimed in claim 1 is characterized in that, dispersion agent is Sudan Gum-arabic in the described the first step, Xylo-Mucine, six segregation sodium phosphates, at least a in the calcium sulfate; Described dispersant dosage is slurry 80～220g per ton.
3. the method for removing carbon impurities in silicon carbide micropowder as claimed in claim 2 is characterized in that, acid is acetic acid in the described the first step, oxalic acid, at least a in 5%～20% the hydrochloric acid.
4. the method for removing carbon impurities in silicon carbide micropowder as claimed in claim 3 is characterized in that, flotation oil is pine camphor oil in described the 4th step, oleic acid, and at least a in the QX-3 flotation oil, the consumption of described flotation oil is slurry 100～160ml per ton.
5. the method for removing carbon impurities in silicon carbide micropowder as claimed in claim 4 is characterized in that, blasting air capacity in described the 4th step is 1600～2300L/h.
6. the method for removing carbon impurities in silicon carbide micropowder as claimed in claim 5 is characterized in that, the hydraulic flotation flow velocity is 1200# silicon carbide micro-powder 420～880L/h in described the 4th step, 1500# silicon carbide micro-powder 180～650L/h.
7. the method for removing carbon impurities in silicon carbide micropowder as claimed in claim 6 is characterized in that, the alkali cleaning medicine is lime in described the 5th step, yellow soda ash, at least a in the water glass.
8. the method for removing carbon impurities in silicon carbide micropowder as claimed in claim 7 is characterized in that, flocculating aids is diatomite in described the 5th step, perlite, medical stone, at least a in the atlapulgite; Described drainage dosage is 4%～12% of stock quality; The granularity of described flocculating aids is 50～150 orders.
9. the method for removing carbon impurities in silicon carbide micropowder as claimed in claim 8 is characterized in that, the oxygen level of the oxidizing atmosphere in described the 6th step is greater than 40%; The drying temperature of described pressure oven dry is 180～220 ℃, and described slurry is dried to water content and is not more than 0.05%.
10. such as the method for the removing carbon impurities in silicon carbide micropowder in any one in the claim 1 to 9, it is characterized in that, centrifugation apparatus is horizontal spiral centrifuge or settling centrifuge in the described second step; Pressure filter is plate and frame(type)filter press in described the 5th step; Forcing the equipment of oven dry in described the 6th step is microwave dryer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101464423A CN102285653B (en) | 2011-06-02 | 2011-06-02 | Method for removing carbon impurities in silicon carbide micropowder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101464423A CN102285653B (en) | 2011-06-02 | 2011-06-02 | Method for removing carbon impurities in silicon carbide micropowder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102285653A CN102285653A (en) | 2011-12-21 |
| CN102285653B true CN102285653B (en) | 2013-04-10 |
Family
ID=45332443
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101464423A Expired - Fee Related CN102285653B (en) | 2011-06-02 | 2011-06-02 | Method for removing carbon impurities in silicon carbide micropowder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102285653B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102923706B (en) * | 2012-11-29 | 2015-04-29 | 江苏乐园新材料集团有限公司 | Preparation method of silicon carbide micro powder capable of improving dispersity |
| CN103950931B (en) * | 2014-05-16 | 2016-02-03 | 宝丰恒瑞新材料有限公司 | A kind for the treatment of process of silicon carbide micro-powder |
| CN106076570B (en) * | 2016-06-14 | 2019-02-05 | 蚌埠玻璃工业设计研究院 | A kind of physical upgrading method realizing feldspar and mica and being separated with quartz |
| CN106698435A (en) * | 2016-12-16 | 2017-05-24 | 苏州金仓合金新材料有限公司 | Silicon carbide particle and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003071205A (en) * | 2001-05-30 | 2003-03-11 | Nippon Steel Corp | Apparatus and method for treating oil stuck particle |
| CN101804983A (en) * | 2010-04-23 | 2010-08-18 | 连云港佳宇电子材料科技有限公司 | Recovery, purification and classification method of high-purity silicon carbide micro-powder |
| CN101823712A (en) * | 2010-04-02 | 2010-09-08 | 河南新大新材料股份有限公司 | Recovery processing method of silicon slice cut waste mortar |
| 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 |
-
2011
- 2011-06-02 CN CN2011101464423A patent/CN102285653B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003071205A (en) * | 2001-05-30 | 2003-03-11 | Nippon Steel Corp | Apparatus and method for treating oil stuck particle |
| CN101823712A (en) * | 2010-04-02 | 2010-09-08 | 河南新大新材料股份有限公司 | Recovery processing method of silicon slice cut waste mortar |
| CN101804983A (en) * | 2010-04-23 | 2010-08-18 | 连云港佳宇电子材料科技有限公司 | Recovery, purification and classification method of high-purity silicon carbide micro-powder |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102285653A (en) | 2011-12-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102285653B (en) | Method for removing carbon impurities in silicon carbide micropowder | |
| EP2349945B1 (en) | Treatment of tailings streams | |
| KR101262408B1 (en) | Process and apparatus for conversion of biomass | |
| CN101804983A (en) | Recovery, purification and classification method of high-purity silicon carbide micro-powder | |
| KR101766928B1 (en) | Method for producing silicon carbide | |
| JP4980793B2 (en) | Silicon recovery method and silicon recovery apparatus | |
| CN110775979B (en) | Method for recovering high-purity silicon and silicon carbide from crystalline silicon cutting waste | |
| CN111116216A (en) | High-utilization-rate regenerated aluminum silicon carbide carbon brick and manufacturing method thereof | |
| WO2011078219A1 (en) | Method for recovering purified silicon-containing powder | |
| CN102923706B (en) | Preparation method of silicon carbide micro powder capable of improving dispersity | |
| CN107162000A (en) | A kind of renovation process of silicon carbide blade material | |
| CN1151893C (en) | Pollution-free gas-phase oxidation separation purification method for artificial diamond | |
| CN102746936A (en) | Recycling purification method for carborundum powder in silicon slice cutting waste liquid | |
| CN1903750A (en) | Circulation reuse method of carbide slag supernatant fluid | |
| CN104449916B (en) | In brown coal, high-concentration coal-water slurry method is prepared in warm upgrading | |
| CN112591757A (en) | Method for preparing white carbon black and sponge copper from organic silicon slurry residues | |
| CN204816912U (en) | Desorption device of free carbon in hierarchical by -product of carborundum miropowder | |
| CN104449917B (en) | High-concentration coal-water slurry method is prepared in the upgrading of brown coal low temperature | |
| CN114655972B (en) | Method for efficiently removing organics from Bayer process alumina solution | |
| CN114317984B (en) | Method for selectively zinc dipping by utilizing cyclone classification-ionic liquid-ultrasonic synergy | |
| CN103663466A (en) | Microbial deferrization process for quartz sand | |
| KR20130034752A (en) | The process of manufacture of molding silicon deoxidizer | |
| CN112341490A (en) | Method for thermochemical treatment and resource utilization of waste glyphosate salt | |
| CN112939178B (en) | Environment-friendly sewage treatment agent for papermaking and production process thereof | |
| JP5522133B2 (en) | Regeneration method of slag |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130410 Termination date: 20160602 |