CN103265033A - Production method of high-purity sub-nanometer silicon carbide micropowder - Google Patents
Production method of high-purity sub-nanometer silicon carbide micropowder Download PDFInfo
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Abstract
The invention relates to a production process of silicon carbide micropower, and in particular relates to a production method of high-purity sub-nanometer silicon carbide micropowder, wherein the D50 value is less than or equal to 1 mu m and the SiC content is greater than or equal to 99.0%. The production method comprises the following steps: casting a silicon carbide micropowder tailing for production line cutting to a fluidized bed airflow mill device; filtering and compressing air; filling water at high pressure and heating to 30kg/cm<2> at 200 DEG C; forming an air flow at 1200m/s by a plurality of nozzles arranged three-dimensionally and injecting to a crushing room, wherein the material is fluidic and the accelerated material reaches ultrafine grinding of particles; conveying the crushed material by rising air flow to a turbine grading area; separating coarse and fine powder under the effect of centrifugal force of a grading wheel and draft of a fan; qualified micropowder meeting the particle request enter into a cyclone grader for further separation and collection along with the air flow and the rest continuously enters into a dedusting system to dedust, while the extremely thin particles are obtained at the outlet of the dedusting system.
Description
Technical field
The present invention relates to a kind of production technique of silicon carbide micro-powder, a kind of preparation D50 value≤1 μ m specifically, the production method of the high-purity sub-nanometer silicon carbide micro powder that SiC content 〉=99.0% is above.
Background technology
High-purity sub-nanometer silicon carbide micro powder is as the raw material of high performance ceramic material, has the characteristic that purity requirement height (SiC content 〉=99.0%), size-grade distribution are wanted refinement (D50 value≤1 μ m), because it has wear-resisting, corrosion-resistant, premium propertiess such as hot strength is high, high thermal conductance, be widely used in high performance structure ceramic material, as absorbing material, anti-wear lubricating grease, high-performance brake facing, the high hardness wear-resisting powder coating, high temperature thermometric protective tube; The used for industrial furnace roller material; The structural ceramics of special purpose, function ceramics, engineering ceramics etc.At present, numerous domestic manufacturer and scientific research institution are forming the orientation test scheme aspect the development of high-purity sub-nanometer silicon carbide micro powder, in stage division, have and in the deionized water of electric conductivity＜100, add micro mist meso-position radius silicon carbide micro-powder, macromolecule dispersing agent is the 2-5% of silicon carbide micro-powder, mixed slurry concentration is that 40-50% sets gradually, and (sees Chinese patent: a kind of production method of silicon carbide micro-powder, application number: 200510047465.3) with this classification that realizes silicon carbide micro-powder; Utilize suspension method, hydraulic classification, material is in the classification jar, intake by the jar bottom, make relative fines be suspended in the classification jar above, after carrying out abundant classification, aspirate out the product of same specification again and (see Chinese patent: a kind of recycling, purifying and classifying technology for high purity superfine silicon carbide micro powder, application number: 200810050205.5); In method of purification, have and at first use alkali cleaning, and then adjust acidity, excessive pickling is adjusted acidity again and is filterer between the 5-6, washing to the ph value, oven dry (is seen Chinese patent: a kind of purification method of ultra fine silicon carbide powder, application number: 200610115158.9); Adopt 10%HCL and 10%H in addition
2SO
4And the 5%NaOH novel process of processing, purification process is through three hypo acid alkali cleanings, and (see Chinese patent: a kind of high purity superfine silicon carbide micro powder reclaims purification techniques, application number: 200810050205.5) in the operation that also needs in the purification process to heat.After having elder generation that slip is carried out stage treatment, in the slip of finishing classification, add deionized water, whipping agent and dispersion agent, with aerator slip is finished physical purification again, carry out chemical purification (see Chinese patent: a kind of method of purification of high-purity sub-nanometer silicon carbide micro powder, application number 201010267587.4) to adding sulfuric acid, hydrochloric acid, hydrofluoric acid, deionized water and alkaline matter in the slip of finishing physical purification then.There is employing that solids is carried out alkali cleaning, pickling and cleaning, obtains silicon carbide slurry and (see Chinese patent: a kind of recovery purification and stage division of high-purity silicon carbide micro-powder, application number: 2010153835.2).Have solid materials is mixed with a certain amount of coke, (see Chinese patent: silicon carbide powder is added method of purification in the silicon chip cutting fluid, application number: 201210279479.8) to be placed in 1500～2000 the atmosphere furnace reaction.
Airflow milling is the energy by high velocity air, makes particle impact mutually, collide, rub and realizes the equipment of superfine grinding.Movement-less part in the airflow milling, easy to maintenance; Adopt totally-enclosed mode, inclusion-free in the production.Produce product and have advantages such as size-grade distribution is good, particle shape is excellent, purity is high, good dispersity.Fluidized bed counter jet mill is with its higher production efficiency and lower wearing and tearing, becomes the preferred manner of high rigidity such as silicon carbide, high-wearing feature material superfine grinding processing.
Summary of the invention
The objective of the invention is to solve the deficiency that exists in the conventional art, provide a kind of by improving processing condition, guarantee the production method of the high-purity sub-nanometer silicon carbide micro powder of product purity.
Technical scheme of the present invention is: a kind of production method of high-purity sub-nanometer silicon carbide micro powder, will produce the silicon carbide micro powder for linear cutting tailing and drop in the fluidized bed counter jet mill equipment, with air after filtration, compression, the high pressure water injection heating reaches 30kg/cm
2, 200 ℃, converge through several nozzles sprays of three-dimensional setting and to form jet velocities and reach the 1200m/s air-flow and inject crushiing chamber, make material be fluidization, the material that is accelerated reaches the superfine grinding of particle; The gas delivery that material after the pulverizing is risen is to the turbine type graded region, and under the effect of grading wheel centrifugal force and blower fan draft, (the thickness powder is to decide according to producing needs in the separation of realization thickness powder.Fine powder is the granularity of producing, meal is the part that surpasses fine powder, needs reprocessing), reach the qualified fine powder of granularity requirements and enter cyclone classifier further separation and collection with air-flow, surplus person continues to enter the dust collecting system dedusting, and superfine person can obtain in the dust collecting system exit.Pulverize feed bin, grading wheel, cyclonic separator and material and all adopted the silicon carbide ceramics lining through pipeline.
Advantage of the present invention is: 1, produce the silicon carbide micro powder for linear cutting tailing and be used for doing raw material for refractory as waste material usually, be used for processing high-purity sub-nanometer silicon carbide micro powder now, by deep processing, form the high added value raw material, energy-conserving and environment-protective, turn waste into wealth, have remarkable economic efficiency and social benefit.2, adopt a kind of disintegrating apparatus, (more than 200 ℃), high pressure (30kg/cm reach a high temperature
2), pollution-free fragmentation, make the disposable desired particle size that is worked into of raw material, need not the later stage stage treatment; solve the problem of classification; can satisfy large-scale industrial production, because in shattering process, entering for totally-enclosed inclusion-free, so the product purity of producing reaches more than 99.0%.3, material is totally-enclosed fragmentation, pulverize feed bin, grading wheel, cyclonic separator and material and all adopted the silicon carbide ceramics lining through pipeline, material prevents from contacting with hardware in shattering process, avoided secondary pollution, inclusion-free participates in, therefore need not to carry out purification processes with sulfuric acid, hydrochloric acid or hydrofluoric acid etc., namely effectively raise production efficiency, stopped the problem of environmental pollution of purification process waste liquid again.4, with the pressurized air heat treated, thereby obtained higher flowed energy; Under the ultrahigh-temperature vapor state, the dynamic collision energy of particle in the fluidized-bed has increased about four times.This makes the production capacity of grinding machine than improving (for portioned product even surpass twice) under the conventional compression air greatly, and the final fineness of tool is also very desirable.
Below in conjunction with accompanying drawing embodiments of the present invention are described in further detail.
Description of drawings
Fig. 1 is operation block diagram of the present invention.
Embodiment
Referring to Fig. 1, a kind of production method raw material of high-purity sub-nanometer silicon carbide micro powder is for producing the tailing (7 μ m～0) of silicon carbide micro powder for linear cutting.Raw material (7 μ m are with thin tailing) carries out fragmentation through disintegrating apparatus, need not to carry out classification, is machined directly to 1 μ m with thin granularity specification, can satisfy large-scale industrial production.Because in shattering process, entering for totally-enclosed inclusion-free, so the product purity of producing reaches more than 99.0%.
Raw material → pulverizing feed bin → cyclonic separator → dust catching device → superfine material reclaims;
Air filtration → pneumatics unit → electric heater → pulverizing feed bin;
Induced draft fan → dust catching device;
Cyclonic separator → finished product.
One, raw material
In producing the silicon carbide micro powder for linear cutting process, can have an appointment 7 μ m more than 10% with thin tailing, this part material processing line cutting with the micro mist process in through common sulfuric acid purification processes, with this part slip with settling vessel centralized collection, oven dry, sieve pine as inferior nano powder raw material (7 μ m～0).
Two, inferior nano ultrafine powders body production technique
Raw material is dropped into disintegrating apparatus, and this equipment is on the basis of fluidized bed counter jet mill principle of work, and (more than 200 ℃), high pressure (30kg/cm reach a high temperature
2), pollution-free fragmentation, make the disposable desired particle size that is worked into of raw material, need not the later stage stage treatment.
Use in the disintegrating apparatus feed bin and prevent secondary pollution technology, need not purification process.Material is totally-enclosed fragmentation, and in shattering process, prevent from contacting with hardware, avoided secondary pollution, inclusion-free participates in, therefore need not to carry out purification processes with sulfuric acid, hydrochloric acid or hydrofluoric acid etc., namely effectively raise production efficiency, stopped the harm problem of purification process environmental pollution and human body again.
The principle of work of equipment be with air after filtration, compression, high pressure water injection heating reaches 30kg/cm
2, 200 ℃, by using high temperature compressed air, the jet velocity of air-flow can reach about 1200m/s; Several nozzle spray remittance formation supersonic airstreams through the three-dimensional setting are injected crushiing chamber, the gas shock that utilizes can make material be fluidization, the material that is accelerated converges at the jet-stream wind joint of several nozzles, produces violent collision, friction, shearing and reaches the superfine grinding of particle.The gas delivery that material after the pulverizing is risen is to the turbine type graded region, under the effect of grading wheel centrifugal force and blower fan draft, realize the separation of thickness powder, when pulverized material is subjected to the promotion of upstream in the crushiing chamber, meal continues pulverizing because crushiing chamber is returned in the action of gravity of self, reach the qualified fine powder of granularity requirements and enter cyclone classifier further separation and collection with air-flow, surplus person continues to enter the dust collecting system dedusting, superfine person can obtain in the dust collecting system exit, and the gas of purification is discharged by induced draft fan.
This equipment with the pressurized air heat treated, thereby has obtained higher flowed energy based on further developing for compressed air on traditional fluidized bed jet mill.In the dry grinding field, reach higher production capacity with this, and extended the fineness scope that dry grinding can obtain.
Under the state of high temperature compressed air, the dynamic collision energy of particle in the fluidized-bed has increased about three times.This makes the production capacity of grinding machine than improving (for portioned product even surpass twice) under the conventional compression air greatly, and the final fineness of tool is also very desirable.The accessible particle diameter cut-point of grading wheel is littler under the conventional compression air condition, and this provides the possibility that obtains littler fineness for us.
When traditional method is carried out fragmentation to raw material, because high rigidity, the high abrasion degree of silicon carbide micro-powder can make common disintegrating apparatus be ground, thereby meeting contaminated material, influence the purity of product, so generally take sulfuric acid, hydrochloric acid or hydrofluoric acid treatment, though removed impurity, environment and human body caused harm.The present invention is for fear of sneak into impurity in shattering process, to pulverizing feed bin, grading wheel, cyclonic separator and material institute through the up-to-date silicon carbide ceramics lining of pipeline employing, utilize its high wear resistance and with raw material, avoided in the past in the equipment shattering process contacting to be worn with hardware causing the material secondary pollution.Therefore, need not to carry out purification processes with sulfuric acid, hydrochloric acid or hydrofluoric acid etc. by adopting this apparatus processing, thereby the production efficiency of effectively raising has been stopped purification process to the pollution of environment and the harm of human body.
After testing: high-purity sub-nanometer silicon carbide micro powder D50 value≤1 μ m, SiC content 〉=more than 99.0%.
Claims (3)
1. the production method of a high-purity sub-nanometer silicon carbide micro powder is characterized in that: will produce the silicon carbide micro powder for linear cutting tailing and drop in the fluidized bed counter jet mill equipment, with air after filtration, compression, heating reaches 30kg/cm
2, 200 ℃, converge through several nozzles sprays of three-dimensional setting and to form jet velocities and reach the 1200m/s air-flow and inject crushiing chamber, make material be fluidization, the material that is accelerated reaches the superfine grinding of particle; The gas delivery that material after the pulverizing is risen is to the turbine type graded region, under the effect of grading wheel centrifugal force and blower fan draft, realize the separation of thickness powder, reach the qualified fine powder of granularity requirements and enter cyclone classifier further separation and collection with air-flow, surplus person continues to enter the dust collecting system dedusting, and superfine person can obtain in the dust collecting system exit.
2. according to the production method of the described high-purity sub-nanometer silicon carbide micro powder of claim 1, it is characterized in that pulverizing feed bin, grading wheel, cyclonic separator and material and all adopted the silicon carbide ceramics lining through pipeline.
3. according to the production method of the described high-purity sub-nanometer silicon carbide micro powder of claim 1, it is characterized in that producing silicon carbide micro powder for linear cutting tailing granularity is 7 μ m～0.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105923659A (en) * | 2016-05-30 | 2016-09-07 | 衢州华友钴新材料有限公司 | Method for preparing battery-grade superfine flaky cobalt hydroxide |
| CN107363263A (en) * | 2017-07-27 | 2017-11-21 | 赣州市钜磁科技有限公司 | A kind of recovery method of waste and old neodymium iron boron |
| WO2021221234A1 (en) * | 2020-04-29 | 2021-11-04 | 주식회사 엘피엔 | Method for manufacturing novel silicon nanoparticles |
| CN115921059A (en) * | 2022-12-27 | 2023-04-07 | 湖南泰通能源管理股份有限公司 | Intelligent compressed air system for anode material and automatic control system of jet mill |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03111527A (en) * | 1989-06-28 | 1991-05-13 | Ibiden Co Ltd | Manufacture of silicon carbide-containing alloy |
| CN2171415Y (en) * | 1993-01-08 | 1994-07-13 | 武汉工业大学 | Compound airfow grinder |
| CN2352257Y (en) * | 1998-12-21 | 1999-12-08 | 上虞市和力粉体有限公司 | Collision type fluidized bed jet mill |
| CN1915541A (en) * | 2006-08-31 | 2007-02-21 | 华南理工大学 | Dry type turbine classifier for micropowder |
| CN101607223A (en) * | 2009-07-06 | 2009-12-23 | 华南理工大学 | A kind of ultra-fine powder processing device |
| CN101941699A (en) * | 2010-09-14 | 2011-01-12 | 东北大学 | Method for reclaiming silicon and silicon carbide from cutting waste materials of monocrystalline silicon and polycrystalline silicon |
| CN102120576A (en) * | 2011-01-25 | 2011-07-13 | 西安通鑫半导体辅料有限公司 | Method for recycling silicon carbide micropowder from waste mortar produced by cutting silicon wafer |
| CN102249236A (en) * | 2011-06-02 | 2011-11-23 | 江苏大阳微粉科技有限公司 | Production process for silicon carbide micropowder |
| CN102351184A (en) * | 2011-07-18 | 2012-02-15 | 矽明科技股份有限公司 | Method for recovering silicon carbide, high-purity silicon and dispersion liquid from silicon material linear cutting waste mortar |
-
2013
- 2013-06-03 CN CN201310215941.2A patent/CN103265033B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03111527A (en) * | 1989-06-28 | 1991-05-13 | Ibiden Co Ltd | Manufacture of silicon carbide-containing alloy |
| CN2171415Y (en) * | 1993-01-08 | 1994-07-13 | 武汉工业大学 | Compound airfow grinder |
| CN2352257Y (en) * | 1998-12-21 | 1999-12-08 | 上虞市和力粉体有限公司 | Collision type fluidized bed jet mill |
| CN1915541A (en) * | 2006-08-31 | 2007-02-21 | 华南理工大学 | Dry type turbine classifier for micropowder |
| CN101607223A (en) * | 2009-07-06 | 2009-12-23 | 华南理工大学 | A kind of ultra-fine powder processing device |
| CN101941699A (en) * | 2010-09-14 | 2011-01-12 | 东北大学 | Method for reclaiming silicon and silicon carbide from cutting waste materials of monocrystalline silicon and polycrystalline silicon |
| CN102120576A (en) * | 2011-01-25 | 2011-07-13 | 西安通鑫半导体辅料有限公司 | Method for recycling silicon carbide micropowder from waste mortar produced by cutting silicon wafer |
| CN102249236A (en) * | 2011-06-02 | 2011-11-23 | 江苏大阳微粉科技有限公司 | Production process for silicon carbide micropowder |
| CN102351184A (en) * | 2011-07-18 | 2012-02-15 | 矽明科技股份有限公司 | Method for recovering silicon carbide, high-purity silicon and dispersion liquid from silicon material linear cutting waste mortar |
Non-Patent Citations (2)
| Title |
|---|
| 董祖龙等: "气流粉碎和分级系统在碳化硅微粉生产中的应用", 《气流粉碎和分级系统在碳化硅微粉生产中的应用》, vol. 7, no. 1, 28 February 2001 (2001-02-28), pages 35 - 37 * |
| 陈海炎: "磨料微粉专用加工系统的研究", 《金刚石与磨料磨具工程》, no. 1, 31 December 2001 (2001-12-31), pages 31 - 33 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105923659A (en) * | 2016-05-30 | 2016-09-07 | 衢州华友钴新材料有限公司 | Method for preparing battery-grade superfine flaky cobalt hydroxide |
| CN107363263A (en) * | 2017-07-27 | 2017-11-21 | 赣州市钜磁科技有限公司 | A kind of recovery method of waste and old neodymium iron boron |
| CN107363263B (en) * | 2017-07-27 | 2019-04-02 | 赣州市钜磁科技有限公司 | A kind of recovery method of waste and old neodymium iron boron |
| WO2021221234A1 (en) * | 2020-04-29 | 2021-11-04 | 주식회사 엘피엔 | Method for manufacturing novel silicon nanoparticles |
| CN115921059A (en) * | 2022-12-27 | 2023-04-07 | 湖南泰通能源管理股份有限公司 | Intelligent compressed air system for anode material and automatic control system of jet mill |
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