CN106542827B - The environment-friendly preparation method thereof of silicon carbide ceramics powder - Google Patents
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Abstract
The invention discloses a kind of environment-friendly preparation method thereofs of silicon carbide ceramics powder, the recycling sand for using solar energy crystal silicon chip cutting waste material to extract is raw material, carry out flotation, grinding, and pass through addition dispersion purification reagent, achieve the purpose that improve slurry dispersibility and imurity-removal, to prepare silicon carbide ceramics powder clean, with high purity.
Description
Technical field
The invention belongs to a kind of preparation methods of silicon carbide micro-powder, and in particular to a kind of fine ceramics silicon carbide micro-powder
Environment-friendly preparation method thereof.
Background technique
Silicon carbide is a kind of important artificial synthesized inorganic non-metallic material, has high rigidity, high-wearing feature, corrosion resistance
And the features such as preferable elevated temperature strength, it is applied in various wear-resisting, corrosion-resistant and resistant to high temperature component of machine.Silicon carbide ceramics
It is that silicon carbide micro-powder is formed through ingredient, molding, normal pressure or reaction-sintered, and silicon carbide has become widely applied ceramic material at present
Material.The raw materials used impurity content of Conventional silicon carbide ceramic powder is high, the removal of impurities preparation process for mostly using soda acid to wash, in preparation process
In need to expend a large amount of soda acid product, environmental pollution is serious.
In addition, the property of ceramic powder directly affects the sintering character and microstructure and mechanical performance of ceramic material, obtain
The sintering ceramic powders that must have excellent properties are the key that production high-performance engineering ceramics.Traditional at present prepares ceramic powder
The method either indexs such as granularity, surface state or purity, uniformity at end, which have been unable to satisfy, increases substantially ceramics
The requirement of performance.
Summary of the invention
For current silicon carbide ceramics powder purity, the larger problem of low, complex manufacturing technology, pollution, the present invention provide one kind
With high purity, environmental-friendly free of contamination silicon carbide ceramics powder, preparation method thereof.
In order to solve the above technical problems, the present invention is with generated cutting waste material in solar energy crystal silicon chip cutting process
Process raw material (cutting waste material be separated by solid-liquid separation be recovered liquid and recycling sand), can be it is a kind of be also possible to a variety of mixtures, both
Cutting waste material can be recycled, and can be improved the purity of raw material.It is realized especially by following technical scheme:
(1) the recycling sand for taking crystal silicon chip cutting waste material is sic raw material, and it is 10 that silicon carbide concentration is added water into raw material
~70wt% stands 10~20min after mixing evenly, removes the impurity swum on liquid level, obtains silicon carbide coarse powder slurry, standby
With；
(2) after mixing evenly by silicon carbide coarse powder slurry obtained by step (1), physical purification is carried out by flotation, by gained
After material grinds 5~15min, flotation is carried out again and strikes off the atrament at liquid level, is then recycled for grinding, flotation
Carbide fine powder slurry is obtained until the D50 that grinding obtains material is 0.5 ± 0.25 μm with the operation for striking off atrament, it is standby
With；
(3) the organic alcohols dispersion purification of its weight 0.1~1% is added into carbide fine powder slurry obtained by step (2)
Agent stands 0.5~72h after mixing evenly, then removes and swims in the impurity of liquid level, repeat add water and stir for carry out 2~5 times,
It stands, remove liquid level impurity；
(4) add water in the slurry that step (3) obtains, and after mixing evenly, stand, precipitating, be then discharged out supernatant, and
Obtained precipitating is subjected to filters pressing, obtains filter cake, it is spare；
(5) filtration cakes torrefaction for obtaining step (4) to moisture content is no more than 0.05wt%, then is crushed, and 3000 mesh are crossed
Strainer to get arrive silicon carbide ceramics powder.
Crystal silicon chip cutting waste material described in above-mentioned steps (1) be preferably in GC#1200, GC#1500, GC#2000 extremely
Few one kind, SiC content therein are not less than 98wt%, D50≤15 μm.
Described with water is preferably conductivity≤80 μ S/cm deionized water.
In the step (2), preferably vertical lapping machine or horizontal mill is ground.
In the step (2), abrasive material used in the process of lapping is preferably aluminium oxide, zirconium oxide, silicon nitride, oxygen
Change at least two kinds of mixing in chromium.
In step (2), abrasive size used in the process of lapping is preferably 0.5~5mm.
In step (3), the organic alcohols dispersion purificant is preferably propyl alcohol, ethylene glycol, glycerine and polyethylene glycol
At least one of.
In step (4), preferably plate and frame type filter-press carries out filters pressing.
The present invention has following positive advantageous effects:
It is concentrated 1. the silicon carbide ceramics Powder Particle Size that the method for the present invention is prepared is distributed, silicon carbide micro-powder granularity shape is neat,
Particle agglomeration is few, and particle dispersion is good, and component is easily controllable, large bulk density.
2. good with slurry fluidity made of silicon carbide ceramics of the present invention, product density is high after sintering porcelain into, 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
Stick, protecting tube, cool air hose, refractory slab, saggar, crucible, blast nozzle and various high temperature resistants, wear-resisting, corrosion-resistant silicon carbide is different
The preparation of type part etc., it is widely used.
3. preparation process is simple, using solar energy crystal silicon chip cutting waste material as raw material, cutting waste material can be recycled to circulation benefit
With, and purity is high, free of contamination silicon carbide ceramics powder can be obtained.
Specific embodiment
Embodiment below facilitates a better understanding of the present invention, but does not limit the present invention.Test in following embodiments
Method is unless otherwise specified conventional method；Raw material as used in the following examples and production equipment, such as without special theory
It is bright, it is commercial product.
Embodiment 1
A kind of environment-friendly preparation method thereof of silicon carbide ceramics powder, includes the following steps:
(1) the recycling sand for taking solar energy crystal silicon chip cutting waste material is raw material, and water (conductivity≤80 μ S/cm is added into raw material
Deionized water), until silicon carbide concentration is 10wt%, stand 20min after mixing evenly, remove the impurity swum on liquid level, obtain
It is spare to silicon carbide coarse powder slurry；Selected solar energy crystal silicon chip cutting waste material is GC#1200, GC#1500, GC#2000's
Mixture, SiC content therein are not less than 98wt%, D50≤15 μm；
(2) after mixing evenly by silicon carbide coarse powder slurry obtained by step (1), physical purification is carried out by flotation, by gained
Material carries out the atrament of flotation and scraper surface again, is then recycled for grinding after vertical lapping machine grinds 5min
Mill, flotation and the operation for striking off atrament obtain carbide fine powder until the D50 that grinding obtains material is 0.5 ± 0.25 μm
Slurry, it is spare；The abrasive size is 0.5~5mm, is mixed for aluminium oxide, zirconium oxide；
(3) the dispersion purificant (propyl alcohol) of its weight 1% is added into carbide fine powder slurry obtained by step (2), stirring is equal
0.5h is stood after even, then removes the impurity for swimming in liquid level, is repeated progress 2 times and is added water and stirred, stands, except liquid level impurity；
(4) add water in the slurry that step (3) obtains, and after mixing evenly, stand, precipitating, be then discharged out supernatant, and
Obtained precipitating is subjected to filters pressing using plate and frame type filter-press, obtains filter cake, it is spare；
(5) filtration cakes torrefaction for obtaining step (4) to moisture content is no more than 0.05wt%, then is crushed, and 3000 mesh are crossed
Strainer is to get silicon carbide ceramics powder is arrived, and detection index of correlation is as follows: 1. carborundum content >=99%；2. even particle size distribution, D50
It is 0.7 ± 0.025 μm；3. total oxygen content≤1.5%.
Embodiment 2
A kind of environment-friendly preparation method thereof of silicon carbide ceramics powder, includes the following steps:
(1) the recycling sand for taking solar energy crystal silicon chip cutting waste material is raw material, and deionized water (conductivity≤80 are added into raw material
μ S/cm) it to silicon carbide concentration is 40wt%, it stands 15min after mixing evenly, removes the impurity swum on liquid level, be carbonized
Silicon coarse powder slurry, it is spare；Selected solar energy crystal silicon chip cutting waste material is GC#2000, and SiC content therein is not less than
98wt%, D50≤15 μm；
(2) after mixing evenly by silicon carbide coarse powder slurry obtained by step (1), physical purification is carried out by flotation, by gained
Material carries out the atrament of flotation and scraper surface again, is then recycled for grinding after vertical lapping machine grinds 10min
Mill, flotation and the operation for striking off atrament obtain carbide fine powder until the D50 that grinding obtains material is 0.5 ± 0.25 μm
Slurry, it is spare；The abrasive size is 0.5~5mm, is mixed for aluminium oxide, silicon nitride；
(3) the dispersion purificant (glycerine) of its weight 0.5% is added into carbide fine powder slurry obtained by step (2), stirs
It is stood after mixing uniformly for 24 hours, then removes the impurity for swimming in liquid level, repeated progress 3 times and add water and stir, stand, except liquid level is miscellaneous
Matter；
(4) add water in the slurry that step (3) obtains, and after mixing evenly, stand, precipitating, be then discharged out supernatant, and
Obtained precipitating is subjected to filters pressing using plate and frame type filter-press, obtains filter cake, it is spare；
(5) filtration cakes torrefaction for obtaining step (4) to moisture content is no more than 0.05wt%, then is crushed, and 3000 mesh are crossed
Strainer is to get silicon carbide ceramics powder is arrived, and detection index of correlation is as follows: 1. carborundum content >=99%；2. even particle size distribution, D50
It is 0.7 ± 0.025 μm；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, includes the following steps:
(1) the recycling sand for taking solar energy crystal silicon chip cutting waste material is raw material, and deionized water (conductivity≤80 are added into raw material
μ S/cm) it to silicon carbide concentration is 70wt%, it stands 10min after mixing evenly, removes the impurity swum on liquid level, be carbonized
Silicon coarse powder slurry, it is spare；Solar energy crystal silicon chip cutting waste material used is GC#1200, SiC content >=98wt% therein, D50
≤15μm；
(2) after mixing evenly by silicon carbide coarse powder slurry obtained by step (1), physical purification is carried out by flotation, by gained
Material carries out the atrament of flotation and scraper surface again, is then recycled for grinding after vertical lapping machine grinds 15min
Mill, flotation and the operation for striking off atrament obtain carbide fine powder until the D50 that grinding obtains material is 0.5 ± 0.25 μm
Slurry, it is spare；The abrasive size is 0.5~5mm, is mixed for silicon nitride, chromium oxide；
(3) the dispersion purificant (polyethylene glycol) of its weight 0.1% is added into carbide fine powder slurry obtained by step (2),
72h is stood after mixing evenly, then removes the impurity for swimming in liquid level, is repeated progress 5 times and is added water and stirred, stands, except liquid level
Impurity；
(4) add water in the slurry that step (3) obtains, and after mixing evenly, stand, precipitating, be then discharged out supernatant, and
Obtained precipitating is subjected to filters pressing using plate and frame type filter-press, obtains filter cake, it is spare；
(5) filtration cakes torrefaction for obtaining step (4) to moisture content is no more than 0.05wt%, then is crushed, and 3000 mesh are crossed
Strainer is to get silicon carbide ceramics powder is arrived, and detection index of correlation is as follows: 1. carborundum content >=99%；2. even particle size distribution, D50
It is 0.7 ± 0.025 μm；3. total oxygen content≤1.5%；4. tap density > 1.99g/cm3.Using the silicon carbide ceramics powder as raw material,
For reaction-sintered at silicon carbide ceramics, main performance indicator is as follows according to a conventional method: 3.07 g/cm of density3, bending strength
515 MPa, 395 GPa of elasticity modulus, thermal expansion coefficient 4.1 × 10-6/℃。
Claims (8)
1. a kind of environment-friendly preparation method thereof of silicon carbide ceramics powder, which comprises the steps of:
(1) choose crystal silicon chip cutting waste material recycling sand be sic raw material, add water to thereto silicon carbide concentration be 10~
70wt% stands 10~20min after mixing evenly, removes the impurity swum on liquid level, obtains silicon carbide coarse powder slurry, spare；
(2) after mixing evenly by silicon carbide coarse powder slurry obtained by step (1), physical purification is carried out by flotation, by resulting material
After grinding 5~15min, flotation is carried out again and strikes off the atrament at liquid level, be then recycled for grinding, flotation and scrape
It is spare except the operation of atrament obtains carbide fine powder slurry until the D50 that grinding obtains material is 0.5 ± 0.25 μm；
(3) organic alcohols that its weight 0.1~1% is added into carbide fine powder slurry obtained by step (2) disperse purificant, stir
Stand 0.5~72h after mixing uniformly, then remove and swim in the impurity of liquid level, repeat add water and stir, stand for carry out 2~5 times,
Except liquid level impurity operates；
(4) add water in the slurry that step (3) obtains, and after mixing evenly, stand, precipitating, be then discharged out supernatant, and incite somebody to action
The precipitating arrived carries out filters pressing, obtains filter cake, spare；
(5) filtration cakes torrefaction for obtaining step (4) to moisture content is no more than 0.05wt%, then is crushed, and the filter of 3000 mesh is crossed
Net to get arrive 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: crystalline substance described in step (1)
Silicon wafer cutting waste material is at least one of 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: the water is conductivity
The deionized water of≤80 μ 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),
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: described in step (2)
Abrasive material used in process of lapping is that aluminium oxide, zirconium oxide, silicon nitride, at least two kinds of 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: described in step (2)
Abrasive size used in process of lapping is 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), described
Organic alcohols dispersion purificant be at least one of propyl alcohol, ethylene glycol, glycerine and polyethylene glycol.
8. the environment-friendly preparation method thereof of silicon carbide ceramics powder according to claim 1, it is characterised in that: in step (4), use
Plate and frame type filter-press carries out filters pressing.
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| 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 |
| CN107010973B (en) * | 2017-05-10 | 2020-05-19 | 济南大学 | Light complex-phase porous heat-insulating refractory material, mullite refractory material and preparation method thereof |
| CN108752003B (en) * | 2018-08-17 | 2021-06-22 | 宁夏和兴碳基材料有限公司 | Preparation method of silicon carbide micro powder for silicon carbide fine ceramic |
| 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 |
| 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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