Content of the invention
It is an object of the invention to avoiding the generation of hollow ball shape particle in silicon carbide granulating powder preparation process.There is provided a kind of
The granulation powder, preparation method thereof of great surface quality silicon carbide mirror can be prepared.
A kind of manufacture method for preparing speculum silicon carbide granulating powder, comprises the following steps, with deionized water as solvent,
Sequentially add carborundum powder, sintering aid, dispersant, plasticiser, binding agent, defoamer to be stirred, through true after stirring
Empty de-bubble, spray drying obtain silicon carbide granulating powder.
Further, described carborundum powder is 1 μm of α-SiC, powder D50 <, purity > 98%.
Further, described sintering aid is B4One or more in C, B or BN are constituted with C, and its addition is carbon
The 1%-10% of SiClx silty amount, is primarily to facilitate the sintering of silicon carbide ceramics, preferably B4The proportioning of C, B or BN and C is (1-
10):(10-1), more preferably (1-6):(6-1), optimum is 4:1.
Further, described dispersant be methyl anyl alcohol, tetramethyl hydrogenation ammonium, the one kind in ethylaminoethanol, its interpolation
The 0.1%-2% for carborundum powder quality is measured, is conducive to silicon carbide powder to be dispersed in solution.
Further, the plasticiser is repefral, di (2-ethylhexyl) phthalate, phthalic acid
One kind in dioctyl ester, its addition are the 1%-15% of carborundum powder quality, increase the plasticity of silicon carbide powder, contribute to powder
Body and the combination of binding agent.
Further, the binding agent be polyvinyl alcohol, polyethylene glycol, the one kind in polyvinyl butyral resin, its interpolation
The 2%-20% for carborundum powder quality is measured, is played during mist projection granulating and powder adhesion spheroiding is acted on.
Further, the defoamer is n-octyl alcohol, polyoxyethylene polyoxypropylene pentaerythrite ether, polyoxyethylene polyoxy third
One kind in alcohol amidogen ether, its addition are the 0.01%-1% of carborundum powder quality, for eliminating the bubble in slurry.
Further, the froth in vacuum process is comprised the following steps:First the ceramic slurry for stirring is placed in very
In empty defoaming machine, vacuum degree control is taken out after keeping 0.5-2 hour in 5-50Pa.
Further, the spray-drying process is comprised the following steps:Adjustment inlet temperature is 220-280 DEG C, outlet temperature
Spend for 75-95 DEG C, atomizer set of frequency is 150-180HZ, air exhauster set of frequency is 40-50HZ, can according to above-mentioned setting
Ensure that moisture controls in 0.7%-1.2% in granulation powder, is conducive to powder dry-pressing formed.
Further, comprise the following steps:1) batch mixing:Appropriate carborundum mill is added to be situated between in vertical mixing mill, carborundum grinds
It is (1.5-3) to be situated between with ceramic slurry mass ratio:1;According to deionized water and sic powder mass ratio (1.2-2):1 add go from
Sub- water and carborundum powder;On the basis of carborundum powder, sintering aid 1%-10%, dispersant 0.1%-2%, defoamer is added
0.01%-1%, starts stirring after mixing.After stirring 1 hour, plasticiser 1%-15% is added, add after continuing stirring 0.5 hour
Enter binding agent 2%-20%, after being stirred for 1 hour, extract slurry out.2) froth in vacuum:The ceramic slurry for stirring is placed in very
In empty defoaming machine, vacuum degree control is taken out after keeping 0.5-2 hour in 5-50Pa.3) it is spray-dried:Adjustment inlet temperature exists
220-280 DEG C, at 75-95 DEG C, in 150-180HZ, air exhauster set of frequency is 40- to atomizer set of frequency to outlet temperature
50HZ.
Further, on the basis of carborundum powder, sintering aid 3%-8%, dispersant 0.5%-1.2%, froth breaking are added
Agent 0.03%-0.6%, starts stirring after mixing.After stirring 1 hour, plasticiser 3%-9.2% is added, continue stirring 0.5 hour
Add binding agent 8%-12% afterwards, after being stirred for 1 hour, extract slurry out.
Further, the silicon carbide granulating powder that a kind of preparation method described above is prepared is provided.
The present invention passes through to add the binding agent of proper proportion, dispersant, plasticiser, defoamer, and froth in vacuum process,
The generation of hollow ball shape particle in silicon carbide granulating powder preparation process is avoided, effectively increases silicon carbide mirror Surface Machining matter
Amount.
Using the method for the invention prepare pelletizing sphericity height (see Fig. 1), even particle size distribution, good fluidity,
Hollow ball shape particle produces few, it is adaptable to the silicon carbide ceramic components that suface processing quality has high demands.Carbonization prepared by the present invention
Silicon pelletizing Hall flow velocity is 2.5s/g, angle of repose:25 ° -26 °, apparent density:0.7-0.8g/cm3, pelletizing D50 are at 55 μm
Left and right.
Other features and advantages of the present invention will be illustrated in the following description, also, partial change from specification
Obtain it is clear that or being understood by implementing the present invention.The purpose of the present invention and other advantages can pass through in the explanation that is write
In book, claims and accompanying drawing, specifically noted structure is realizing and obtain.
Embodiment 1:
A kind of manufacture method for preparing speculum silicon carbide granulating powder, comprises the following steps:
1) batch mixing:Appropriate silicon carbide ceramics mill is added to be situated between in vertical mixing mill, silicon carbide ceramics mill is situated between and ceramic slurry matter
Amount is than being 2:1;According to deionized water and sic powder mass ratio 1.6:1 adds deionized water and carborundum powder;With carborundum
On the basis of powder, B is added4Mixture 5%, the tetramethyl hydrogenation ammonium 1% of C, B and C, n-octyl alcohol 0.1%, start stirring after mixing.
After stirring 1 hour, di (2-ethylhexyl) phthalate 6% is added, polyethylene glycol 10% after continuing stirring 0.5 hour, is added, then
Stirring extracted slurry out after 1 hour.
2) froth in vacuum:The ceramic slurry for stirring is placed in froth in vacuum machine, vacuum degree control is kept in 20Pa
Take out after 1 hour.
3) it is spray-dried:Adjustment inlet temperature at 250 DEG C, outlet temperature at 90 DEG C, atomizer set of frequency in 160HZ,
Air exhauster set of frequency is 45HZ.
According to above-mentioned preparation process, pelletizing sphericity height, even particle size distribution, good fluidity, hollow ball shape is obtained
Particle produces few silicon carbide granulating powder.The silicon carbide granulating powder Hall flow velocity of preparation is 2.5s/g, angle of repose:25 ° -26 °, pine
Dress density:0.7-0.8g/cm3, pelletizing D50 are at 55 μm or so.
Embodiment 2:
A kind of manufacture method for preparing speculum silicon carbide granulating powder, comprises the following steps:
1) batch mixing:Appropriate silicon carbide ceramics mill is added to be situated between in vertical mixing mill, silicon carbide ceramics mill is situated between and ceramic slurry matter
Amount is than being 2.5:1;According to deionized water and sic powder mass ratio 1.8:1 adds deionized water and carborundum powder;With carbonization
On the basis of silica flour, B is added4The mixture 6.8% of C, B and C, ethylaminoethanol 1.1%, polyoxyethylene polyoxypropylene pentaerythrite
Ether 0.25%, starts stirring after mixing.After stirring 1 hour, dioctyl phthalate 12% is added, continue stirring 0.5 hour
Add polyvinyl butyral resin 13.5% afterwards, after being stirred for 1 hour, extract slurry out.
2) froth in vacuum:The ceramic slurry for stirring is placed in froth in vacuum machine, vacuum degree control is kept in 10Pa
Take out after 2 hours.
3) it is spray-dried:Adjustment inlet temperature at 230 DEG C, outlet temperature at 85 DEG C, atomizer set of frequency in 170HZ,
Air exhauster set of frequency is 40HZ.
According to above-mentioned preparation process, pelletizing sphericity height, even particle size distribution, good fluidity, hollow ball shape is obtained
Particle produces few silicon carbide granulating powder.The silicon carbide granulating powder Hall flow velocity of preparation is 2.5s/g, angle of repose:25 ° -26 °, pine
Dress density:0.7-0.8g/cm3, pelletizing D50 are at 55 μm or so.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, the change or replacement that can readily occur in,
Should all be included within the scope of the present invention.