Summary of the invention
In view of this, be necessary to be directed against the problem that background technology is mentioned, provide a kind of and improve product planeness, surface quality, and reduce the preparation method of the tabular alumina pottery of gauge fluctuation.
The present invention realizes through following technical scheme:
A kind of coating preparation method of tabular alumina pottery, it may further comprise the steps:
It is that 60 ~ 70% alumina powders, mass percent are that 15 ~ 25% organic solvent, mass percent are that 0.61 ~ 2.92% solubility promoter, mass percent are that 0.4 ~ 1.5% dispersion agent, mass percent are that 3.0 ~ 5.0% sticker, mass percent are 2.0 ~ 6.0% softening agent that mass percent is provided;
Said solubility promoter was ground 4 ~ 8 hours and mixed with sand mill in advance; Said solubility promoter is joined ball mill dry grinded 2 ~ 4 hours with said alumina powder; Again said organic solvent stirring and dissolving in impeller of dispersion agent and 50% quality was joined in the ball mill ball milling 6 ~ 24 hours after 1 ~ 2 hour; In this process, said sticker and said softening agent are joined in the said organic solvent of other 50% quality in impeller stirring and dissolving and joined in the ball mill ball milling after 4 ~ 10 hours again 24 ~ 48 hours;
With the slurry that the prepares deaeration under-0.05 ~ 1Mpa vacuum condition in the ball mill, but obtain the slurry that coated and molded is used after stirring reaches 10000 ~ 30000mps simultaneously;
But said coated and molded is injected traditional curtain coating shaper with slurry; Regulate scraper and spacing, scraper and the film band speed of relative movement of film band and the difference of altitude of slurry liquid level and film band; Get the green compact of thickness 0.15 ~ 2.0mm after the warm air drying; Pass through die-cut, 24 ~ 48 hours the low temperature binder removal of mould again, obtain the tabular alumina pottery behind 1400 ~ 1700 ℃ of high temperature sinterings of 12 ~ 24 hours.
The diameter of said alumina powder is 0.5 ~ 8.0um.
Said organic solvent adopts binary azeotropic mixed organic solvents system, and like Virahol and ETHYLE ACETATE, both mass ratios are 1:3; This system can provide good dissolution characteristics, and solvent can have good chemicalstability with constant component evaporation, and not with powder generation chemical reaction, the slurry of preparation is nontoxic simultaneously, and cost is low.
Said dispersion agent adopts two kinds of ceramic dispersants, and like Viscotrol C and poly carboxylic acid, both mass ratios are 2 ~ 3:1; Because both dispersing propertys are different; Promptly the adsorptive power to ceramic grain surface is different; Single dispersion agent causes the dispersing property extremalization easily, causes the continuous deterioration of blank cracking after the moulding or size performance, and therefore two kinds of dispersion agents are that moulding process provides stable performance significant.
Said sticker adopts two kinds of stickers: two kinds of different polyvinyl butyral acetals (PVB) that molecular chain length is short with molecular chain, and both mass ratios are 1 ~ 3:1; The molecular chain of different lengths promptly has different molecular weight, and the PVB of molecular chain length provides the base band strength, and molecular chain short PVB provide intergranular viscosity in the base band, and two kinds of stickers use optimizes the slurry viscosity, and flowability strengthens blank strength and cementability etc.
Said softening agent adopts two kinds of softening agent: polyoxyethylene glycol (PEG) and Witcizer 300 (DBP), both mass ratio=1:1 ~ 1.5; The base band of two kinds of softening agent preparations of experiment proof is not easy to crack, snappiness is moderate.
For the tabular alumina pottery of big specification, the mode of static pressure such as employing temperature guarantees its planeness, and concrete technology is; Be placed in the smooth mould large stretch of green compact and the bag film of packing into, plastic packaging under the vacuum of-0.1Mpa is put into isostatic pressing machine; Under 70 ~ 95 ℃ temperature, evenly suppress green compact with 15 ~ 25Mpa pressure, take out again after the cooling; Make big specification green density each to being tending towards evenly, thereby guarantee the planeness of tabular alumina pottery behind the sintering.
Also can adopt multilayer stack isostatic pressing method to obtain the tabular alumina pottery of big specification good planeness.
Green compact behind the shaping and drying are cut into band shape through cutting knife and batch, and it is old more than 24 hours to put into old storehouse, process the dimensions that needs through punching press, cut-out, punching etc.; Behind dusting machine dusting, put into low temperature binder removal stove after 4 ~ 8 stacks again, with 5 ~ 10 ℃/minute speed binder removal; The dispersion agent that slowly adds in the decomposition prescription, sticker, softening agent etc.; The time that binder removal needs is directly proportional with the size of green compact, guarantees that the green compact behind the binder removal do not ftracture, and is indeformable.
Green compact behind the binder removal are put into the push-plate type electric furnace again, heat up with 3 ~ 5 ℃/minute speed, and lowering the temperature naturally after 2 ~ 5 hours 1600 ~ 1700 ℃ of insulations obtains the tabular alumina pottery, and oxide platelet pottery generally speaking is sintering in air directly.
A kind of concrete implementation method is:
The following mixture of proportion raw material by mass percentage is provided:
Diameter is the alumina powder of 0.9 ~ 5.0um: 66.2%;
Mass ratio as solubility promoter is Natural manganese dioxide, silicon oxide and the lime carbonate of 2:1:0.5: totally 2.76%;
Mass ratio as organic solvent is Virahol and the ETHYLE ACETATE of 1:3: totally 23.5%;
Mass ratio as dispersion agent is Viscotrol C and the poly carboxylic acid of 3:1: totally 0.966%;
Mass ratio as sticker is PVB-long-chain and the PVB-short chain of 2:1: totally 3.93%;
Mass ratio as softening agent is DBP and the PEG of 1:1: totally 2.62%;
Earlier the fusing assistant in the powder was ground 6 hours and mixed with sand mill in advance; It is joined ball mill dry grinded 2 hours, more said organic solvent stirring and dissolving in impeller of dispersion agent and 50% quality was joined in the ball mill ball milling 12 hours after 1.5 hours with powder; The organic solvent stirring and dissolving in impeller that in this process, sticker and softening agent is joined other 50% quality joined in the ball mill ball milling 32 hours again after 10 hours; The slurry for preparing need be in deaeration under the-0.1Mpa vacuum condition, obtains the slurry that coated and molded is used but stir simultaneously after reaching 20000mps;
Then, said slurry is injected a curtain coating shaper, scraper and film interband distance are adjusted into 2.5mm; Slurry liquid level and film band difference of altitude are adjusted into 40mm; Scraper and film band speed of relative movement are adjusted into 0.25m/min, behind the hot air drier inner drying of 30 ~ 110 ℃ of temperature, obtain the green compact of thickness 1.18mm, and it is die-cut to pass through mould again; In 90 ℃ warm water; Obtain green compact under the pressure with 20Mpa,, obtain the tabular alumina pottery of thickness 1mm behind 14 hours 1600 ℃ the high temperature sintering through 24 hours low temperature binder removal.
Another kind of concrete implementation method is:
The following mixture of proportion raw material by mass percentage is provided:
Diameter is the alumina powder of 0.9 ~ 5.0um: 65.2%;
Mass ratio as solubility promoter is Natural manganese dioxide, lime carbonate and the yttrium oxide of 3:2:1: totally 0.659%;
Mass ratio as organic solvent is Virahol and the ETHYLE ACETATE of 1:3: totally 25.7%;
Mass ratio as dispersion agent is Viscotrol C and the poly carboxylic acid of 2:1: totally 1.19%;
Mass ratio as sticker is PVB-long-chain and the PVB-short chain of 2:1: totally 4.28%;
Mass ratio as softening agent is DBP and the PEG of 2:1: totally 2.96%;
Earlier the fusing assistant in the powder was ground 8 hours and mixed with sand mill in advance; It is joined ball mill dry grinded 4 hours, again organic solvent stirring and dissolving in impeller of dispersion agent and 50% quality was joined in the ball mill ball milling 18 hours after 1.3 hours with powder; The organic solvent stirring and dissolving in impeller that in this process, sticker and softening agent is joined other 50% quality joined in the ball mill ball milling 40 hours again after 12 hours; The slurry for preparing need be in deaeration under the-0.1Mpa vacuum condition, obtains the slurry that coated and molded is used but stir simultaneously after reaching 22000mps;
Then, said slurry is injected a curtain coating shaper, scraper and film interband distance are adjusted into 2.2mm; Slurry liquid level and film band difference of altitude are 40mm; Scraper and film band speed of relative movement are adjusted into 0.25m/min, behind the hot air drier inner drying of 30 ~ 110 ℃ of temperature, obtain the green compact of thickness 1.20mm, and it is die-cut to pass through mould again; In 90 ℃ warm water; Obtain green compact under the pressure with 22Mpa,, obtain the tabular alumina pottery of thickness 1mm behind 18 hours 1690 ℃ the high temperature sintering through 26 hours low temperature binder removal.
Compared with prior art, the present invention possesses following advantage:
1, adopt binary azeotropic mixed organic solvents system, like Virahol and ETHYLE ACETATE, both mass ratios are 1:3; This system can provide good dissolution characteristics; And solvent can have good chemicalstability, not with powder generation chemical reaction with the evaporation of constant component; The slurry of preparation is nontoxic simultaneously, and cost is low;
2, adopt two kinds of ceramic dispersants, like Viscotrol C and poly carboxylic acid, both mass ratios are 2 ~ 3:1; Because both dispersing propertys are different; Promptly the adsorptive power to ceramic grain surface is different; Single dispersion agent causes the dispersing property extremalization easily, causes the continuous deterioration of blank cracking after the moulding or size performance, and therefore two kinds of dispersion agents are that moulding process provides stable performance significant;
3, adopt two kinds of stickers: two kinds of different polyvinyl butyral acetals (PVB) that molecular chain length is short with molecular chain, both mass ratios are 1 ~ 3:1; The molecular chain of different lengths promptly has different molecular weight, and the PVB of molecular chain length provides the base band strength, and molecular chain short PVB provide intergranular viscosity in the base band, and two kinds of stickers use optimizes the slurry viscosity, and flowability strengthens blank strength and cementability etc.;
4, adopt two kinds of softening agent: polyoxyethylene glycol (PEG) and Witcizer 300 (DBP), both mass ratio=1:1 ~ 1.5; The base band of two kinds of softening agent preparations of experiment proof is not easy to crack, snappiness is moderate.
Embodiment
Embodiment one, the mass percent of aluminum oxide is 96% aluminum oxide sheet ceramic preparation:
Fill a prescription as follows:
Title |
Composition |
Weight |
Alumina powder |
Diameter is 0.9 ~ 5.0um |
960kg |
Fusing assistant |
Natural manganese dioxide: silicon oxide: lime carbonate=2:1:0.5 |
40kg |
Organic solvent |
Virahol: ETHYLE ACETATE=1:3 |
340kg |
Dispersion agent |
Viscotrol C: poly carboxylic acid=3:1 |
14kg |
Sticker |
PVB-long-chain: PVB-short chain=2:1 |
57kg (U.S. first promise company produces) |
Softening agent |
DBP:PEG=1:1 |
38kg |
The preparation method is:
Earlier the fusing assistant in the powder was ground 6 hours and mixed with sand mill in advance; It is joined ball mill dry grinded 2 hours, again organic solvent stirring and dissolving in impeller of dispersion agent and 50% quality was joined in the ball mill ball milling 12 hours after 1.5 hours with powder; The organic solvent stirring and dissolving in impeller that in this process, sticker and softening agent is joined other 50% quality joined in the ball mill ball milling 32 hours again after 10 hours; The slurry for preparing need be in deaeration under the-0.1Mpa vacuum condition, obtains the slurry that coated and molded is used but stir simultaneously after reaching 20000mps;
Then, but the slurry that said coated and molded is used is injected a curtain coating shaper, scraper and film interband distance are adjusted into 2.5mm with clearance gauge; Slurry liquid level and film band difference of altitude are 40mm; Scraper and film band speed of relative movement are adjusted into 0.25m/min, behind the hot air drier inner drying of 30 ~ 110 ℃ of temperature, obtain the green compact of thickness 1.18mm, and it is die-cut to pass through mould again; In 90 ℃ warm water; Obtain green compact under the pressure with 20Mpa,, obtain the tabular alumina pottery of thickness 1mm behind 14 hours 1600 ℃ the high temperature sintering through 24 hours low temperature binder removal.
96% aluminum oxide sheet ceramic performance such as the following table that obtains:
Performance project |
Performance index |
Performance project |
Performance index |
Volume density |
3.74g/cm3 |
Water-intake rate |
0% |
Bending strength |
325Mpa |
Dielectric strength |
13KV/mm |
Linear expansivity |
6.8*10-6mm/℃ |
Specific inductivity |
10(1MHz) |
Roughness |
Ra=0.25um |
Dielectric loss |
3*10-4(1MHz) |
Heat-shock resistance |
Do not split for 7 times from 850 ℃ of chillings |
Planeness |
(0.2/100 length direction) |
Embodiment two: the mass percent of aluminum oxide is 99% aluminum oxide sheet ceramic preparation:
Fill a prescription as follows:
Title |
Composition |
Weight |
Alumina powder |
Diameter is 0.9 ~ 5.0um |
990kg |
Fusing assistant |
3:2:1=Natural manganese dioxide: lime carbonate: yttrium oxide |
10kg |
Organic solvent |
Virahol: ETHYLE ACETATE=1:3 |
390kg |
Dispersion agent |
Viscotrol C: poly carboxylic acid=2:1 |
18kg |
Sticker |
PVB-long-chain: PVB-short chain=2:1 |
65kg (U.S. first promise company produces) |
Softening agent |
DBP:PEG=1.2:1 |
45kg |
The preparation method is:
Earlier the fusing assistant in the powder was ground 8 hours and mixed with sand mill in advance; It is joined ball mill dry grinded 4 hours, again organic solvent stirring and dissolving in impeller of dispersion agent and 50% quality was joined in the ball mill ball milling 18 hours after 1.3 hours with powder; The organic solvent stirring and dissolving in impeller that in this process, sticker and softening agent is joined other 50% quality joined in the ball mill ball milling 40 hours again after 12 hours.The slurry for preparing need be in deaeration under the-0.1Mpa vacuum condition, obtains the slurry that coated and molded is used but stir simultaneously after reaching 22000mps;
But the slurry that said coated and molded is used is injected a curtain coating shaper; With clearance gauge scraper and film interband distance are adjusted into 2.2mm, slurry liquid level and film band difference of altitude are 40mm, and scraper and film band speed of relative movement are adjusted into 0.25m/min; Behind the hot air drier inner drying of 30 ~ 110 ℃ of temperature, obtain the green compact of thickness 1.20mm; It is die-cut to pass through mould again, in 90 ℃ warm water, obtains green compact under the pressure with 22Mpa; Through 26 hours low temperature binder removal, obtain the tabular alumina pottery of thickness 1mm behind 18 hours 1690 ℃ the high temperature sintering.
99% aluminum oxide sheet ceramic performance such as the following table that obtains:
Performance project |
Performance index |
Performance project |
Performance index |
Volume density |
3.90g/cm3 |
Water-intake rate |
0% |
Bending strength |
>350Mpa |
Dielectric strength |
18KV/mm |
Linear expansivity |
7.2~8*10-6mm/℃ |
Specific inductivity |
10(1MHz) |
Roughness |
Ra=0.22um |
Dielectric loss |
2*10-4(1MHz) |
Thermal conductivity |
>25(W/m.K) |
Planeness |
(0.2/100 length direction) |
The present invention has the following advantages
1, adopt binary azeotropic mixed organic solvents system, like Virahol and ETHYLE ACETATE, both mass ratios are 1:3; This system can provide good dissolution characteristics; And solvent can have good chemicalstability, not with powder generation chemical reaction with the evaporation of constant component; The slurry of preparation is nontoxic simultaneously, and cost is low;
2, adopt two kinds of ceramic dispersants, like Viscotrol C and poly carboxylic acid, both mass ratios are 2 ~ 3:1; Because both dispersing propertys are different; Promptly the adsorptive power to ceramic grain surface is different; Single dispersion agent causes the dispersing property extremalization easily, causes the continuous deterioration of blank cracking after the moulding or size performance, and therefore two kinds of dispersion agents are that moulding process provides stable performance significant;
3, adopt two kinds of stickers: two kinds of different polyvinyl butyral acetals (PVB) that molecular chain length is short with molecular chain, both mass ratios are 1 ~ 3:1; The molecular chain of different lengths promptly has different molecular weight, and the PVB of molecular chain length provides the base band strength, and molecular chain short PVB provide intergranular viscosity in the base band, and two kinds of stickers use optimizes the slurry viscosity, and flowability strengthens blank strength and cementability etc.;
4, adopt two kinds of softening agent: polyoxyethylene glycol (PEG) and Witcizer 300 (DBP), both mass ratio=1:1 ~ 1.5; The base band of two kinds of softening agent preparations of experiment proof is not easy to crack, snappiness is moderate.