CN106542827A - The environment-friendly preparation method thereof of silicon carbide ceramics powder - Google Patents
The environment-friendly preparation method thereof of silicon carbide ceramics powder Download PDFInfo
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- CN106542827A CN106542827A CN201610930079.7A CN201610930079A CN106542827A CN 106542827 A CN106542827 A CN 106542827A CN 201610930079 A CN201610930079 A CN 201610930079A CN 106542827 A CN106542827 A CN 106542827A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
The invention discloses a kind of environment-friendly preparation method thereof of silicon carbide ceramics powder, the recovery sand that solar energy crystal silicon chip cutting waste material is extracted is adopted for raw material, carry out flotation, grinding, and by adding dispersion purification reagent, the purpose for improving slurry dispersiveness and imurity-removal is reached, the silicon carbide ceramics powder high so as to prepare clean, purity.
Description
Technical field
The invention belongs to a kind of preparation method of silicon carbide micro-powder, and in particular to a kind of fine ceramics silicon carbide micro-powder
Environment-friendly preparation method thereof.
Background technology
Carborundum is a kind of important artificial synthesized Inorganic Non-metallic Materials, with high rigidity, high-wearing feature, corrosion resistance
And the features such as preferable elevated temperature strength, be applied in various wear-resisting, corrosion-resistant and resistant to elevated temperatures components of machine.Silicon carbide ceramics
It is that silicon carbide micro-powder Jing dispensings, shaping, normal pressure or reaction-sintered are formed, and carborundum has become wide variety of ceramic material at present
Material.The raw materials used impurity content of Conventional silicon carbide ceramic powder is high, the removal of impurities preparation technology for being washed using soda acid more, in preparation process
In need to expend substantial amounts of soda acid product, environmental pollution is serious.
Additionally, the property of ceramic powder directly affects the sintering character and microstructure and mechanical performance of ceramic material, obtain
The sintering ceramic powders must with excellent properties are the keys for making high-performance engineering ceramics.Traditional at present prepares ceramic powder
Method either granularity, the surface state at end, or the index such as purity, uniformity cannot meet and increase substantially ceramics
The requirement of performance.
The content of the invention
For current silicon carbide ceramics powder purity is low, complex manufacturing technology, larger problem is polluted, the present invention provides a kind of
Purity is high, the free of contamination silicon carbide ceramics powder, preparation method thereof of environmental friendliness.
In order to solve above technical problem, the present invention with the cutting waste material produced by solar energy crystal silicon chip cutting process is
Process raw material（Cutting waste material separation of solid and liquid is recovered liquid and reclaims sand）, can be it is a kind of can also be various compounds, both
Cutting waste material recycle and reuse can be improved the purity of raw material again.Realize especially by technical scheme below：
（1）The recovery sand for taking crystal silicon chip cutting waste material is sic raw material, add water to in raw material silicon carbide concentration for 10～
70wt%, stands 10～20min after stirring, removing swims in the impurity on liquid level, obtains carborundum meal slip, standby；
（2）By step（1）After gained carborundum meal slip stirs, physical purification is carried out by flotation, by resulting material
After 5～15min of grinding, flotation is carried out again and the atrament at liquid level is struck off, be then recycled for grinding, flotation and scrape
Except the operation of atrament, until the D50 that grinding obtains material is 0.5 ± 0.25 μm, carbide fine powder slip is obtained, it is standby；
（3）To step（2）The dispersion purificant of its weight 0.1～1% is added in gained carbide fine powder slip, after stirring
0.5～72h is stood, is then removed and is swum in the impurity of liquid level, repeated and carry out 2～5 stirrings that add water, standing, except liquid level is miscellaneous
Matter；
（4）In step（3）Add water in the slip for obtaining, and after stirring, stand, precipitate, be then discharged out supernatant, and incite somebody to action
To precipitation carry out press filtration, obtain filter cake, it is standby；
（5）By step（4）The filtration cakes torrefaction for obtaining is less than 0.05wt% to moisture, then is crushed, and crosses the filter of 3000 mesh
Net, that is, obtain silicon carbide ceramics powder.
Above-mentioned steps（1）Described crystal silicon chip cutting waste material preferably in GC#1200, GC#1500, GC#2000 extremely
Few one kind, SiC content therein are not less than 98wt%, D50≤15 μm.
The deionized water that electrical conductivity≤80 S/cm is preferably with water.
In the step（2）In, preferred vertical lapping machine or horizontal mill are ground.
In the step（2）In, Preferred abrasives are aluminum oxide, zirconium oxide, silicon nitride, at least 2 kinds mixing in chromium oxide
Form.
In step（2）In, described abrasive size is preferably 0.5～5mm.
In step（3）In, the dispersion purificant preferably organic alcohols reagent is propyl alcohol, ethylene glycol, glycerine and is gathered
At least one in ethylene glycol.
In step（4）In, preferred plate and frame type filter-press carries out press filtration.
The present invention has following positive Advantageous Effects：
1. the silicon carbide ceramics Powder Particle Size distribution that the inventive method is prepared is concentrated, and silicon carbide micro-powder granularity shape is neat, particle
Reunite few, particle dispersion is good, and component is easily controllable, and bulk density is big.
2. good with slurry fluidity made by silicon carbide ceramics of the present invention, after sintering porcelain into, product density is high, the anti-folding of high temperature
Property is excellent, can be used for ceramic kiln furniture, high temperature bocca, fluid delivery device, radiant tube and leads flame set, desulfurization nozzle, crossbeam, roller
Rod, protecting tube, cool air hose, refractory slab, saggar, crucible, blast nozzle and various high temperature resistants, wear-resisting, corrosion-resistant carborundum are different
The preparation of type part etc., it is of many uses.
3. cutting waste material, with solar energy crystal silicon chip cutting waste material as raw material, can be reclaimed circulation profit by preparation process is simple
With can obtain that purity is high, free of contamination silicon carbide ceramics powder again.
Specific embodiment
Below example facilitates a better understanding of the present invention, but does not limit the present invention.Test in following embodiments
Method, if no special instructions, is conventional method；Raw material used and production equipment in following embodiments, such as without special theory
It is bright, it is commercially available prod.
Embodiment 1
A kind of environment-friendly preparation method thereof of silicon carbide ceramics powder, comprises the steps：
（1）The recovery sand for taking solar energy crystal silicon chip cutting waste material is raw material, is added water in raw material（Electrical conductivity≤80 S/cm's goes
Ionized water）, it is 10wt% to silicon carbide concentration, after stirring, stands 20min, removing swims in the impurity on liquid level, obtains carbon
SiClx meal slip, it is standby；Mixing of the selected solar energy crystal silicon chip cutting waste material for GC#1200, GC#1500, GC#2000
Material, SiC content therein are not less than 98wt%, D50≤15 μm；
（2）By step（1）After gained carborundum meal slip stirs, physical purification is carried out by flotation, by resulting material
Jing after vertical lapping machine grinding 5min, the atrament of flotation scraper surface is carried out again, is then recycled for grinding, floated
The operation of atrament is selected and is struck off, until the D50 that grinding obtains material is 0.5 ± 0.25 μm, carbide fine powder slip is obtained,
It is standby；Described abrasive size is 0.5～5mm, is that aluminum oxide, zirconium oxide are mixed；
（3）To step（2）The dispersion purificant of its weight 1% is added in gained carbide fine powder slip（Propyl alcohol）, after stirring
0.5h is stood, is then removed and is swum in the impurity of liquid level, repeated and carry out 2 stirrings that add water, standing, except liquid level impurity；
（4）In step（3）Add water in the slip for obtaining, and after stirring, stand, precipitate, be then discharged out supernatant, and incite somebody to action
To precipitation press filtration is carried out using plate and frame type filter-press, obtain filter cake, it is standby；
（5）By step（4）The filtration cakes torrefaction for obtaining is less than 0.05wt% to moisture, then is crushed, and crosses the filter of 3000 mesh
Net, that is, obtain silicon carbide ceramics powder, and detection index of correlation is as follows：1. carborundum content >=99%；2. even particle size distribution, D50For
0.7±0.025μm；3. total oxygen content≤1.5%.
Embodiment 2
A kind of environment-friendly preparation method thereof of silicon carbide ceramics powder, comprises the steps：
（1）The recovery sand for taking solar energy crystal silicon chip cutting waste material is raw material, adds deionized water in raw material（Electrical conductivity≤80 S/
cm）It is 40wt% to silicon carbide concentration, after stirring, stands 15min, removing swims in the impurity on liquid level, obtains carborundum
Meal slip, it is standby；Selected solar energy crystal silicon chip cutting waste material be GC#2000, SiC content therein be not less than 98wt%,
D50≤15μm；
（2）By step（1）After gained carborundum meal slip stirs, physical purification is carried out by flotation, by resulting material
Jing after vertical lapping machine grinding 10min, carry out the atrament of flotation scraper surface again, be then recycled for grinding,
Flotation and the operation of atrament is struck off, until the D50 that grinding obtains material is 0.5 ± 0.25 μm, obtain carbide fine powder material
Slurry, it is standby；Described abrasive size is 0.5～5mm, is that aluminum oxide, silicon nitride are mixed；
（3）To step（2）The dispersion purificant of its weight 0.5% is added in gained carbide fine powder slip（Glycerine）, stirring is
24h is stood after even, is then removed and is swum in the impurity of liquid level, repeated and carry out 3 stirrings that add water, standing, except liquid level impurity；
（4）In step（3）Add water in the slip for obtaining, and after stirring, stand, precipitate, be then discharged out supernatant, and incite somebody to action
To precipitation press filtration is carried out using plate and frame type filter-press, obtain filter cake, it is standby；
（5）By step（4）The filtration cakes torrefaction for obtaining is less than 0.05wt% to moisture, then is crushed, and crosses the filter of 3000 mesh
Net, that is, obtain silicon carbide ceramics powder, and detection index of correlation is as follows：1. carborundum content >=99%；2. even particle size distribution, D50For
0.7±0.025μm；3. total oxygen content≤1.5%；4. tap density ＞ 1.97g/cm3。
Embodiment 3
A kind of environment-friendly preparation method thereof of silicon carbide ceramics powder, comprises the steps：
（1）The recovery sand for taking solar energy crystal silicon chip cutting waste material is raw material, adds deionized water in raw material（Electrical conductivity≤80 S/
cm）It is 70wt% to silicon carbide concentration, after stirring, stands 10min, removing swims in the impurity on liquid level, obtains carborundum
Meal slip, it is standby；Solar energy crystal silicon chip cutting waste material used be GC#1200, SiC content >=98wt% therein, D50≤
15μm；
（2）By step（1）After gained carborundum meal slip stirs, physical purification is carried out by flotation, by resulting material
Jing after vertical lapping machine grinding 15min, carry out the atrament of flotation scraper surface again, be then recycled for grinding,
Flotation and the operation of atrament is struck off, until the D50 that grinding obtains material is 0.5 ± 0.25 μm, obtain carbide fine powder material
Slurry, it is standby；Described abrasive size is 0.5～5mm, is that silicon nitride, chromium oxide are mixed；
（3）To step（2）The dispersion purificant of its weight 0.1% is added in gained carbide fine powder slip（Polyethylene glycol）, stirring
72h is stood after uniform, the impurity for swimming in liquid level is then removed, is repeated and is carried out 5 stirrings that add water, standing, except liquid level impurity；
（4）In step（3）Add water in the slip for obtaining, and after stirring, stand, precipitate, be then discharged out supernatant, and incite somebody to action
To precipitation press filtration is carried out using plate and frame type filter-press, obtain filter cake, it is standby；
（5）By step（4）The filtration cakes torrefaction for obtaining is less than 0.05wt% to moisture, then is crushed, and crosses the filter of 3000 mesh
Net, that is, obtain silicon carbide ceramics powder, and detection index of correlation is as follows：1. carborundum content >=99%；2. even particle size distribution, D50For
0.7±0.025μm；3. total oxygen content≤1.5%；4. tap density ＞ 1.99g/cm3.With the silicon carbide ceramics powder as raw material, press
, into silicon carbide ceramics, its main performance indications is as follows for conventional method reaction-sintered：3.07 g/cm of density3, bending strength 515
MPa, 395 GPa of elastic modelling quantity, thermal coefficient of expansion 4.1 × 10-6/℃。
Claims (9)
1. a kind of environment-friendly preparation method thereof of silicon carbide ceramics powder, it is characterised in that comprise the steps：
（1）The recovery sand for choosing crystal silicon chip cutting waste material is sic raw material, add water to thereto silicon carbide concentration for 10～
70wt%, stands 10～20min after stirring, removing swims in the impurity on liquid level, obtains carborundum meal slip, standby；
（2）By step（1）After gained carborundum meal slip stirs, physical purification is carried out by flotation, by resulting material
After 5～15min of grinding, flotation is carried out again and the atrament at liquid level is struck off, be then recycled for grinding, flotation and scrape
Except the operation of atrament, until the D50 that grinding obtains material is 0.5 ± 0.25 μm, carbide fine powder slip is obtained, it is standby；
（3）To step（2）The dispersion purificant of its weight 0.1～1% is added in gained carbide fine powder slip, after stirring
0.5～72h is stood, is then removed and is swum in the impurity of liquid level, repeated and carry out 2～5 stirrings that add water, standing, except liquid level is miscellaneous
Matter is operated；
（4）In step（3）Add water in the slip for obtaining, and after stirring, stand, precipitate, be then discharged out supernatant, and incite somebody to action
To precipitation carry out press filtration, obtain filter cake, it is standby；
（5）By step（4）The filtration cakes torrefaction for obtaining is less than 0.05wt% to moisture, then is crushed, and crosses the filter of 3000 mesh
Net, that is, obtain silicon carbide ceramics powder.
2. the environment-friendly preparation method thereof of silicon carbide ceramics powder according to claim 1, it is characterised in that：Step（1）Described crystalline substance
Silicon chip cutting waste material is at least one in GC#1200, GC#1500, GC#2000, and SiC content therein is not less than 98wt%,
D50≤15μm。
3. the environment-friendly preparation method thereof of silicon carbide ceramics powder according to claim 1, it is characterised in that：Described water is electrical conductivity
The deionized water of≤80 S/cm.
4. the environment-friendly preparation method thereof of silicon carbide ceramics powder according to claim 1, it is characterised in that：In the step（2）In,
It is ground by vertical lapping machine or horizontal mill.
5. the environment-friendly preparation method thereof of silicon carbide ceramics powder according to claim 1, it is characterised in that：In step（2）In, it is described
Abrasive material be aluminum oxide, zirconium oxide, silicon nitride, at least 2 kinds in chromium oxide mix.
6. the environment-friendly preparation method thereof of silicon carbide ceramics powder according to claim 1, it is characterised in that：In step（2）In, it is described
Abrasive size be 0.5～5mm.
7. the environment-friendly preparation method thereof of silicon carbide ceramics powder according to claim 1, it is characterised in that：In step（3）In, it is described
Dispersion purificant be organic alcohols reagent.
8. the environment-friendly preparation method thereof of silicon carbide ceramics powder according to claim 7, it is characterised in that：Described organic alcohols examination
Agent is at least one in propyl alcohol, ethylene glycol, glycerine and polyethylene glycol.
9. the environment-friendly preparation method thereof of silicon carbide ceramics powder according to claim 1, it is characterised in that：In step（4）In, adopt
Plate and frame type filter-press carries out press filtration.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106946576A (en) * | 2017-04-12 | 2017-07-14 | 潮州三环（集团）股份有限公司 | A kind of method that ceramic powder is prepared with ceramic solid waste |
| CN107010973A (en) * | 2017-05-10 | 2017-08-04 | 济南大学 | A kind of lightweight complex phase porous heat-insulating refractory material and mullite refractory and preparation method thereof |
| CN108752003A (en) * | 2018-08-17 | 2018-11-06 | 宁夏和兴碳基材料有限公司 | The preparation method of silicon carbide fine ceramics silicon carbide micro-powder |
| CN108996506A (en) * | 2018-09-25 | 2018-12-14 | 内蒙古华鑫硅材料科技有限公司 | A kind of method of crystal silicon chip recycling waste material ball |
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| 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 |
| CN103496831A (en) * | 2013-09-18 | 2014-01-08 | 河南新大新材料股份有限公司 | Recycling method of silicon wafer cutting edge material waste water treatment sludge |
| CN105129801A (en) * | 2015-07-16 | 2015-12-09 | 河南新大新材料股份有限公司 | Recycle and reuse method of by-product from production of silicon carbide |
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| 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 |
| CN103496831A (en) * | 2013-09-18 | 2014-01-08 | 河南新大新材料股份有限公司 | Recycling method of silicon wafer cutting edge material waste water treatment sludge |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106946576A (en) * | 2017-04-12 | 2017-07-14 | 潮州三环（集团）股份有限公司 | A kind of method that ceramic powder is prepared with ceramic solid waste |
| CN107010973A (en) * | 2017-05-10 | 2017-08-04 | 济南大学 | A kind of lightweight complex phase porous heat-insulating refractory material and mullite refractory and preparation method thereof |
| CN108752003A (en) * | 2018-08-17 | 2018-11-06 | 宁夏和兴碳基材料有限公司 | The preparation method of silicon carbide fine ceramics silicon carbide micro-powder |
| CN108996506A (en) * | 2018-09-25 | 2018-12-14 | 内蒙古华鑫硅材料科技有限公司 | A kind of method of crystal silicon chip recycling waste material ball |
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