CN102718498B - Coating preparation method for flakey aluminum oxide ceramic - Google Patents
Coating preparation method for flakey aluminum oxide ceramic Download PDFInfo
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Abstract
The invention provides a coating preparation method for flakey aluminum oxide ceramic, which comprises the following steps of: providing 60-70wt% of alumina powder material, 15-25wt% of organic solvent, 0.61-2.92wt% of cosolvent, 0.4-1.5wt% of dispersing agent, 3.0-5.0wt% of binding agent and 2.0-6.0wt% of plasticizer, wherein the organic solvent adopts a binary azeotropy mixing organic solvent system, such as isopropanol and ethyl acetate; two dispersing agents are adopted, such as castor oil and polycarboxylic acid; the binding agent adopts two different polyvinyl butyral (PVB) with a short molecular chain and a short molecular chain; and the plasticizer adopts polyethylene glycol (PEG) and dibutyl phthalate (DBP). The flakey aluminum oxide ceramic prepared with the coating preparation method disclosed by the invention has the advantages of good evenness and surface quality and small thickness size fluctuation, and the quality requirement of a subsequent printing circuit can be satisfied.
Description
Technical field
The present invention relates to the electronic ceramics technical field, be specifically related to a kind of coating preparation method of tabular alumina pottery.
Background technology
The pottery of sheet is widely used in the strut member of printer bar, LED cooling base, electronic component, thick film and thin film circuit, piezoelectric ceramics diaphragm and electrical condenser diaphragm etc.Because the overwhelming majority in the non-water base moulding process of current making tabular alumina pottery adopts single dispersion agent, single binding agent and single softening agent, adopt product planeness, the surface quality of its explained hereafter relatively poor, the gauge fluctuation is large, can't satisfy the specification of quality of follow-up printed wiring.
Summary of the invention
In view of this, being necessary provides the problem mentioned for background technology a kind of and improves product planeness, surface quality, and reduces the preparation method of the tabular alumina pottery of gauge fluctuation.
The present invention is achieved by the following technical solutions:
A kind of coating preparation method of tabular alumina pottery, it comprises the following 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% binding agent, mass percent are 2.0 ~ 6.0% softening agent that mass percent is provided;
Described solubility promoter was ground 4 ~ 8 hours and mixed with sand mill in advance; Described solubility promoter is joined ball mill dry grinded 2 ~ 4 hours together with described alumina powder; Again described organic solvent stirring and dissolving in homogenizer of dispersion agent and 50% quality was joined in ball mill ball milling after 1 ~ 2 hour 6 ~ 24 hours; Described binding agent and described softening agent are joined in the described organic solvent of other 50% quality in homogenizer stirring and dissolving in this process and joined again in ball mill ball milling after 4 ~ 10 hours 24 ~ 48 hours;
With the slurry that the prepares deaeration under-0.05 ~ 1Mpa vacuum condition in ball mill, but obtain the slurry that coated and molded is used after stirring reaches 10000 ~ 30000mps simultaneously;
But described coated and molded is injected traditional curtain coating forming machine 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 warm air drying, pass through again that mould is die-cut, the low temperature binder removal of 24 ~ 48 hours, obtain the tabular alumina pottery after 1400 ~ 1700 ℃ of high temperature sinterings of 12 ~ 24 hours.
The diameter of described alumina powder is 0.5 ~ 8.0um.
Described organic solvent adopts binary azeotropic mixed organic solvents system, and as Virahol and ethyl acetate, both mass ratios are 1:3; This system can provide good dissolution characteristics, and solvent can have good chemical stability with the evaporation of constant component, and not with powder generation chemical reaction, the slurry of preparation is nontoxic simultaneously, and cost is low.
Described dispersion agent adopts two kinds of ceramic dispersants, and as Viscotrol C and poly carboxylic acid, both mass ratios are 2 ~ 3:1; Because both dispersing propertys are different, namely the adsorptive power to ceramic grain surface is different, single dispersion agent easily causes the dispersing property extremalization, causes the continuous deterioration of blank cracking after moulding or size performance, and therefore two kinds of dispersion agents provide stable performance significant for moulding process.
Described binding agent adopts two kinds of binding agents: two kinds of different polyvinyl butyral acetals (PVB) that molecular chain length and molecular chain are short, and both mass ratios are 1 ~ 3:1; The molecular chain of different lengths namely has different molecular weight, and the PVB of molecular chain length provides the base band strength, and the short PVB of molecular chain provides intergranular viscosity in the base band, and two kinds of binding agents use optimizes slurry viscosity, and mobility strengthens blank strength and cementability etc.
Described softening agent adopts two kinds of softening agent: polyoxyethylene glycol (PEG) and dibutyl phthalate (DBP), both mass ratio=1:1 ~ 1.5; The base band that experimental results show that the preparation of two kinds of softening agent is not easy to crack, snappiness is moderate.
Tabular alumina pottery for large specification, adopt temperature to wait the mode of static pressure to guarantee its planeness, concrete technology is, is placed in smooth mould large stretch of green compact and the bag film of packing into, plastic packaging under the vacuum of-0.1Mpa, put into isostatic pressing machine, at the temperature of 70 ~ 95 ℃, evenly suppress green compact with 15 ~ 25Mpa pressure, take out again after cooling, make large specification green density each to being tending towards evenly, thereby guarantee the planeness of sheet alumina-ceramic after sintering.
Also can adopt the multiple-layer stacked isostatic pressing method to obtain the good tabular alumina pottery of large specification planeness.
Green compact after shaping and drying are cut into band shape by cutting knife and batch, put into old storehouse old more than 24 hours, make the dimensions that needs through punching press, cut-out, punching etc., after the powder-coating machine dusting, then put into the low temperature draft glue discharging furnace after 4 ~ 8 stacks, with the speed binder removal of 5 ~ 10 ℃/minute, the dispersion agent that slowly adds in the decomposition formula, binding agent, softening agent etc., the time that binder removal needs is directly proportional to the size of green compact, guarantees that the green compact after binder removal do not ftracture, and is indeformable.
Green compact after binder removal are put into the push-plate type electric furnace again, heat up with the speed of 3 ~ 5 ℃/minute, and naturally lowering the temperature after 2 ~ 5 hours 1600 ~ 1700 ℃ of insulations obtains the tabular alumina pottery, and oxide platelet pottery generally is sintering in air directly.
A kind of concrete implementation method is:
The raw mix of following proportioning by mass percentage is provided:
Diameter is the alumina powder of 0.9 ~ 5.0um: 66.2%;
Mass ratio as solubility promoter is magnesium oxide, silicon oxide and the calcium carbonate of 2:1:0.5: totally 2.76%;
Mass ratio as organic solvent is Virahol and the ethyl 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 binding agent 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%;
First the fusing assistant in powder was ground 6 hours and mixed with sand mill in advance, it is joined ball mill dry grinded together with powder 2 hours, more described organic solvent stirring and dissolving in homogenizer of dispersion agent and 50% quality was joined in ball mill ball milling 12 hours after 1.5 hours; The organic solvent stirring and dissolving in homogenizer that binding agent and softening agent is joined other 50% quality in this process joined in ball mill ball milling 32 hours again after 10 hours; The slurry for preparing need to be in deaeration under-0.1Mpa vacuum condition, obtains the slurry that coated and molded is used but stir simultaneously after reaching 20000mps;
Then, described slurry is injected a curtain coating forming machine, scraper and film band spacing 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, obtain the green compact of thickness 1.18mm after the hot air drier inner drying of 30 ~ 110 ℃ of temperature, pass through again mould die-cut, in the warm water of 90 ℃, obtain green compact under pressure with 20Mpa, through the low temperature binder removal of 24 hours, obtain the tabular alumina pottery of thickness 1mm after the high temperature sintering of 1600 ℃ of 14 hours.
Another kind of concrete implementation method is:
The raw mix of following proportioning by mass percentage is provided:
Diameter is the alumina powder of 0.9 ~ 5.0um: 65.2%;
Mass ratio as solubility promoter is magnesium oxide, calcium carbonate and the yttrium oxide of 3:2:1: totally 0.659%;
Mass ratio as organic solvent is Virahol and the ethyl 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 binding agent 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%;
First the fusing assistant in powder was ground 8 hours and mixed with sand mill in advance, it is joined ball mill dry grinded together with powder 4 hours, then organic solvent stirring and dissolving in homogenizer of dispersion agent and 50% quality was joined in ball mill ball milling 18 hours after 1.3 hours; The organic solvent stirring and dissolving in homogenizer that binding agent and softening agent is joined other 50% quality in this process joined in ball mill ball milling 40 hours again after 12 hours; The slurry for preparing need to be in deaeration under-0.1Mpa vacuum condition, obtains the slurry that coated and molded is used but stir simultaneously after reaching 22000mps;
Then, described slurry is injected a curtain coating forming machine, scraper and film band spacing 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, obtain the green compact of thickness 1.20mm after the hot air drier inner drying of 30 ~ 110 ℃ of temperature, pass through again mould die-cut, in the warm water of 90 ℃, obtain green compact under pressure with 22Mpa, through the low temperature binder removal of 26 hours, obtain the tabular alumina pottery of thickness 1mm after the high temperature sintering of 1690 ℃ of 18 hours.
Compared with prior art, the present invention possesses following advantage:
1, adopt binary azeotropic mixed organic solvents system, as Virahol and ethyl acetate, both mass ratios are 1:3, this system can provide good dissolution characteristics, and solvent can with constant component evaporation, have good chemical stability, not with powder generation chemical reaction, the slurry of preparation is nontoxic simultaneously, and cost is low;
2, adopt two kinds of ceramic dispersants, as Viscotrol C and poly carboxylic acid, both mass ratios are 2 ~ 3:1; Because both dispersing propertys are different, namely the adsorptive power to ceramic grain surface is different, single dispersion agent easily causes the dispersing property extremalization, causes the continuous deterioration of blank cracking after moulding or size performance, and therefore two kinds of dispersion agents provide stable performance significant for moulding process;
3, adopt two kinds of binding agents: two kinds of different polyvinyl butyral acetals (PVB) that molecular chain length and molecular chain are short, both mass ratios are 1 ~ 3:1; The molecular chain of different lengths namely has different molecular weight, and the PVB of molecular chain length provides the base band strength, and the short PVB of molecular chain provides intergranular viscosity in the base band, and two kinds of binding agents use optimizes slurry viscosity, and mobility strengthens blank strength and cementability etc.;
4, adopt two kinds of softening agent: polyoxyethylene glycol (PEG) and dibutyl phthalate (DBP), both mass ratio=1:1 ~ 1.5; The base band that experimental results show that the preparation of two kinds of softening agent 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 | Magnesium oxide: silicon oxide: calcium carbonate=2:1:0.5 | 40kg |
| Organic solvent | Virahol: ethyl acetate=1:3 | 340kg |
| Dispersion agent | Viscotrol C: poly carboxylic acid=3:1 | 14kg |
| Binding agent | PVB-long-chain: PVB-short chain=2:1 | The 57kg(U.S. first promise company produces) |
| Softening agent | DBP:PEG=1:1 | 38kg |
The preparation method is:
First the fusing assistant in powder was ground 6 hours and mixed with sand mill in advance, it is joined ball mill dry grinded together with powder 2 hours, then organic solvent stirring and dissolving in homogenizer of dispersion agent and 50% quality was joined in ball mill ball milling 12 hours after 1.5 hours; The organic solvent stirring and dissolving in homogenizer that binding agent and softening agent is joined other 50% quality in this process joined in ball mill ball milling 32 hours again after 10 hours; The slurry for preparing need to be in deaeration under-0.1Mpa vacuum condition, obtains the slurry that coated and molded is used but stir simultaneously after reaching 20000mps;
Then, but the slurry that described coated and molded is used is injected a curtain coating forming machine, with clearance gauge, scraper and film band spacing are adjusted into 2.5mm, 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, obtain the green compact of thickness 1.18mm after the hot air drier inner drying of 30 ~ 110 ℃ of temperature, pass through again mould die-cut, in the warm water of 90 ℃, obtain green compact under pressure with 20Mpa, through the low temperature binder removal of 24 hours, obtain the tabular alumina pottery of thickness 1mm after the high temperature sintering of 1600 ℃ of 14 hours.
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=magnesium oxide: calcium carbonate: yttrium oxide | 10kg |
| Organic solvent | Virahol: ethyl acetate=1:3 | 390kg |
| Dispersion agent | Viscotrol C: poly carboxylic acid=2:1 | 18kg |
| Binding agent | PVB-long-chain: PVB-short chain=2:1 | The 65kg(U.S. first promise company produces) |
| Softening agent | DBP:PEG=1.2:1 | 45kg |
The preparation method is:
First the fusing assistant in powder was ground 8 hours and mixed with sand mill in advance, it is joined ball mill dry grinded together with powder 4 hours, then organic solvent stirring and dissolving in homogenizer of dispersion agent and 50% quality was joined in ball mill ball milling 18 hours after 1.3 hours; The organic solvent stirring and dissolving in homogenizer that binding agent and softening agent is joined other 50% quality in this process joined in ball mill ball milling 40 hours again after 12 hours.The slurry for preparing need to be in deaeration under-0.1Mpa vacuum condition, obtains the slurry that coated and molded is used but stir simultaneously after reaching 22000mps;
But the slurry that described coated and molded is used is injected a curtain coating forming machine, with clearance gauge, scraper and film band spacing 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, obtain the green compact of thickness 1.20mm after the hot air drier inner drying of 30 ~ 110 ℃ of temperature, pass through again mould die-cut, in the warm water of 90 ℃, obtain green compact under pressure with 22Mpa, through the low temperature binder removal of 26 hours, obtain the tabular alumina pottery of thickness 1mm after the high temperature sintering of 1690 ℃ of 18 hours.
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, as Virahol and ethyl acetate, both mass ratios are 1:3, this system can provide good dissolution characteristics, and solvent can with constant component evaporation, have good chemical stability, not with powder generation chemical reaction, the slurry of preparation is nontoxic simultaneously, and cost is low;
2, adopt two kinds of ceramic dispersants, as Viscotrol C and poly carboxylic acid, both mass ratios are 2 ~ 3:1; Because both dispersing propertys are different, namely the adsorptive power to ceramic grain surface is different, single dispersion agent easily causes the dispersing property extremalization, causes the continuous deterioration of blank cracking after moulding or size performance, and therefore two kinds of dispersion agents provide stable performance significant for moulding process;
3, adopt two kinds of binding agents: two kinds of different polyvinyl butyral acetals (PVB) that molecular chain length and molecular chain are short, both mass ratios are 1 ~ 3:1; The molecular chain of different lengths namely has different molecular weight, and the PVB of molecular chain length provides the base band strength, and the short PVB of molecular chain provides intergranular viscosity in the base band, and two kinds of binding agents use optimizes slurry viscosity, and mobility strengthens blank strength and cementability etc.;
4, adopt two kinds of softening agent: polyoxyethylene glycol (PEG) and dibutyl phthalate (DBP), both mass ratio=1:1 ~ 1.5; The base band that experimental results show that the preparation of two kinds of softening agent is not easy to crack, snappiness is moderate.
Claims (3)
1. the coating preparation method of a tabular alumina pottery is characterized in that: comprise the following steps:
It is that 60～70% alumina powders, mass percent are that 15～25% organic solvent, mass percent are that 0.61～2.92% fusing assistant, mass percent are that 0.4～1.5% dispersion agent, mass percent are that 3.0～5.0% binding agent, mass percent are 2.0～6.0% softening agent that mass percent is provided;
Described fusing assistant was ground 4～8 hours and mixed with sand mill in advance; Described fusing assistant is joined ball mill dry grinded 2～4 hours together with described alumina powder; Again described organic solvent stirring and dissolving in homogenizer of dispersion agent and 50 quality % was joined in ball mill ball milling after 1～2 hour 6～24 hours; Described binding agent and described softening agent are joined in the described organic solvent of other 50 quality % in homogenizer stirring and dissolving in this process and joined again in ball mill ball milling after 4～10 hours 24～48 hours;
With the slurry that the prepares deaeration under-0.05～1Mpa vacuum condition in ball mill, but obtain the slurry that coated and molded is used after stirring reaches 10000～30000mps simultaneously;
But described coated and molded is injected traditional curtain coating forming machine 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 warm air drying, pass through again that mould is die-cut, the low temperature binder removal of 24～48 hours, obtain the tabular alumina pottery after 1400～1700 ℃ of high temperature sinterings of 12～24 hours;
The diameter of described alumina powder is 0.5～8.0um; Described fusing assistant comprises two or more in magnesium oxide, silicon oxide, yttrium oxide and calcium carbonate; Described organic solvent comprises that mass ratio is Virahol and the ethyl acetate of 1:3; Described dispersion agent comprises that mass ratio is Viscotrol C and the poly carboxylic acid of 2～3:1; Described binding agent comprises that mass ratio is two kinds of binding agents of 1～3:1: two kinds of different polyvinyl butyral acetals that molecular chain length and molecular chain are short; Described softening agent adopts two kinds of softening agent: polyoxyethylene glycol and dibutyl phthalate, both mass ratioes are 1:1～1.5.
2. method according to claim 1 is characterized in that: comprise the following steps:
The raw mix of following proportioning by mass percentage is provided:
Diameter is the alumina powder of 0.9～5.0um: 66.2%;
Mass ratio as fusing assistant is magnesium oxide, silicon oxide and the calcium carbonate of 2:1:0.5: totally 2.76%;
Mass ratio as organic solvent is Virahol and the ethyl 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 binding agent 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%;
First the fusing assistant in powder was ground 6 hours and mixed with sand mill in advance, it is joined ball mill dry grinded together with powder 2 hours, more described organic solvent stirring and dissolving in homogenizer of dispersion agent and 50% quality was joined in ball mill ball milling 12 hours after 1.5 hours; The organic solvent stirring and dissolving in homogenizer that binding agent and softening agent is joined other 50% quality in this process joined in ball mill ball milling 32 hours again after 10 hours; The slurry for preparing need to be in deaeration under-0.1Mpa vacuum condition, obtains the slurry that coated and molded is used but stir simultaneously after reaching 20000mps;
Then, but the slurry that described coated and molded is used is injected a curtain coating forming machine, with clearance gauge, scraper and film band spacing are adjusted into 2.5mm, 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, obtain the green compact of thickness 1.18mm after the hot air drier inner drying of 30～110 ℃ of temperature, pass through again mould die-cut, in the warm water of 90 ℃, obtain green compact under pressure with 20Mpa, through the low temperature binder removal of 24 hours, obtain the tabular alumina pottery of thickness 1mm after the high temperature sintering of 1600 ℃ of 14 hours.
3. method according to claim 1 is characterized in that: comprise the following steps:
The raw mix of following proportioning by mass percentage is provided:
Diameter is the alumina powder of 0.9～5.0um: 65.2%;
Mass ratio as fusing assistant is magnesium oxide, calcium carbonate and the yttrium oxide of 3:2:1: totally 0.659%;
Mass ratio as organic solvent is Virahol and the ethyl 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 binding agent 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%;
First the fusing assistant in powder was ground 8 hours and mixed with sand mill in advance, it is joined ball mill dry grinded together with powder 4 hours, then organic solvent stirring and dissolving in homogenizer of dispersion agent and 50% quality was joined in ball mill ball milling 18 hours after 1.3 hours; The organic solvent stirring and dissolving in homogenizer that binding agent and softening agent is joined other 50% quality in this process joined in ball mill ball milling 40 hours again after 12 hours; The slurry for preparing need to be in deaeration under-0.1Mpa vacuum condition, obtains the slurry that coated and molded is used but stir simultaneously after reaching 22000mps;
then, but the slurry that described coated and molded is used is injected a curtain coating forming machine, with clearance gauge, scraper and film band spacing 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, obtain the green compact of thickness 1.20mm after the hot air drier inner drying of 30～110 ℃ of temperature, pass through again mould die-cut, in the warm water of 90 ℃, obtain the tabular alumina ceramic green under pressure with 22Mpa, low temperature binder removal through 26 hours, obtain the tabular alumina pottery of thickness 1mm after the high temperature sintering of 1690 ℃ of 18 hours.
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| CN101269977B (en) * | 2008-05-04 | 2010-11-10 | 景德镇陶瓷学院 | Method for preparing ceramic sheet with composite caking agent series water-based cast |
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