CN101870577B - Preparation method of magnesium phase-enriched cordierite water-based tape casting slurry - Google Patents
Preparation method of magnesium phase-enriched cordierite water-based tape casting slurry Download PDFInfo
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- CN101870577B CN101870577B CN 201010209508 CN201010209508A CN101870577B CN 101870577 B CN101870577 B CN 101870577B CN 201010209508 CN201010209508 CN 201010209508 CN 201010209508 A CN201010209508 A CN 201010209508A CN 101870577 B CN101870577 B CN 101870577B
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Abstract
The invention discloses a preparation method of magnesium phase-enriched cordierite water-based tape casting slurry, which comprises the following components by mass percent: 15-35% of cordierite, 8-18% of sodium polyacrylate solution, 30-40% of polyvinyl alcohol solution, 5-10% of polyethylene glycol solution and 10-40% of ultrapure water. The preparation method comprises the following steps of: 1, adding cordierite powder into the ultrapure water, uniformly stirring, then adding the sodium polyacrylate solution, and continuously stirring to emulsion slurry; 2, placing the emulsion slurry into a zirconia ball-milling tank, taking zirconia ball-milling stones as ball-milling medium, ball milling for six hours at the first time, and obtaining a primary slurry; 3, adding the polyvinyl alcohol solution and the polyethylene glycol solution into the primary slurry, ball milling for 16-18 hours at the second time, and obtaining cordierite water-based tape casting slurry; 4, vacuum bubble removing for 30-60 minutes at the room temperature; and 5, sealed standing for 15-30 minutes at the room temperature, and then obtaining the magnesium phase-enriched cordierite water-based tape casting slurry. The invention has no pollution, low cost, simple preparation technology, low organic content and good film formation performance.
Description
Technical field
The present invention relates to a kind of aqueous casting slurry and preparation method thereof, particularly magnesium phase-enriched cordierite (2MgO-2Al
2O
3-5SiO
2) aqueous casting slurry and preparation method thereof, belong to the casting technique field.
Background technology
Trichroite (2MgO-2Al
2O
3-5SiO
2) base ceramic material is owing to have good dielectric properties, lower thermal expansivity and lower sintering temperature, is considered to one of very promising electronic material.High-purity, high reactivity magnesium phase-enriched cordierite that sol-gel method makes can make the green compact of moulding separate out the a-trichroite under lower sintering temperature.
Be applied to the trichroite (2MgO-2Al of power electronics industrial circle in order to obtain all kinds
2O
3-5SiO
2) electronic devices and components, mainly adopt casting method to its moulding.Flow casting molding (tape-casitgn also claims Dcoot-bladign or Kinef-coaitgn) is a kind of important moulding process of thin slice stupalith.In casting molding processes, the most important thing is that technique is the preparation of slurry.
The preparation of slurry mainly is divided into two kinds: a kind of is the preparation of slurry in traditional casting molding processes, and a kind of is the preparation of slurry in the aqueous tape casting forming technique.
Prepare shortcoming maximum in the trichroite slurry process at traditional casting technique and be that with an organic solvent (such as toluene, dimethylbenzene etc.) are as solution, not only make slurry system have toxicity, produce the objectionable impurities of a large amount of contaminate environment in the production, and production cost is higher.In addition, these organism major parts all are inflammable substance (such as acetone etc.), also can produce a large amount of potential safety hazards aborning.The characteristics that water-based flow casting technique prepares trichroite slurry maximum are to adopt water to make solvent, solved that the parts of traditional casting molding processes leaves over such as problems such as production cost are high, seriously polluted, but aqueous tape casting forming technique also has the deficiency of himself: because tackiness agent dispersion agent that can be simultaneously water-soluble is few, therefore select narrow, the weak effect of tackiness agent range of choice, see at present the report tackiness agent and only have latex, PVA and celluosic resin, dispersion agent then only has polyacrylic acid (PAA) and ammonium polymethacrylate (PMMA) etc.; Water is large as the solvent surface tension, and boiling point is high, therefore relatively poor to the powder wettability, volatilization is slow and time of drying is long, slurry also easily produces bubble in mechanical milling process, need adding defrother and tensio-active agent, and need exhaust air technique; Slurry character is responsive to processing parameter, is difficult for the fine and close smooth ceramic membrane of molded surface, is difficult to obtain the consistence product; Selective to ceramic powder, can not prepare and can close with the steeping in water for reconstitution unboiled water ceramic powder raw cook of reaction.
In sum, in the preparation of trichroite slurry, mainly there is following problem:
1, adopt traditional casting technique to prepare slurry more, pollute greatly, cost is high.
2, dispersion agent can not be water-soluble, is not suitable for water-based tape casting, needs to cooperate the PH conditioning agent to use, and experimentation is complicated.
3, need to add defrother in the de-bubble process, increased organic usage quantity.
4, the green compact release property is poor in the curtain coating process, and demould time is long, and is easy to crack.
Summary of the invention
By the preparation method of a kind of magnesium phase-enriched cordierite water-based tape casting slurry provided by the present invention, this slurry is pollution-free, and cost is low, and preparation technology is simple, and organic content is low, good film-forming property.
A kind of magnesium phase-enriched cordierite water-based tape casting slurry provided by the invention, its component and mass percent are: trichroite 15%～35%, sodium polyacrylate solution 8%～18%, polyvinyl alcohol solution 30%～40%, polyglycol solution 5%～10%, ultrapure water 10%～40%; The sodium polyacrylate solution concentration 4% of using, the concentration of polyvinyl alcohol solution are 5%, and polyglycol solution concentration is 17%.
The preparation method of a kind of magnesium phase-enriched cordierite water-based tape casting slurry that the present invention proposes may further comprise the steps:
1, be that to join massfraction be in 10%～40% the ultrapure water to 15%～35% cordierite powder with massfraction, glass stick stirs, ultrapure water is the sodium polyacrylate solution that adds massfraction 8%～18% behind the loose Heshui state in cordierite powder, continue to stir into the emulsus slurry.
2, the emulsus slurry in the step 1 is inserted in the zirconia ball grinding jar, take the zirconia ball mill as ball-milling medium, ball milling 6 hours for the first time in planetary comprehensive ball mill obtains elementary slurry.
3, be that 30%～40% polyvinyl alcohol solution, massfraction are that 5%～10% polyglycol solution adds in the elementary slurry that step 2 obtains with massfraction, ball milling 16～18 hours for the second time in planetary comprehensive ball mill, obtain cordierite water-based tape casting slurry, solid content is 15%～35%.
4, the cordierite water-based tape casting slurry that the second time, ball milling obtained is placed on the froth in vacuum machine, froth in vacuum is 30～60 minutes under the room temperature.
5, at room temperature, with the cordierite water-based tape casting slurry sealing and standing after the froth in vacuum 15～30 minutes, then namely obtain a kind of magnesium phase-enriched cordierite water-based tape casting slurry.
The present invention compared with prior art has following features:
1, makes water as solvent, eliminated the environmental pollution that with an organic solvent causes, can greatly reduce production costs.
2, adopt sodium polyacrylate as dispersion agent, do not need to regulate the pH value of slurry, simplify the technological process of slurry preparation.
3, de-bubble process does not need to add defoamer can obtain slurry uniform and stable, that have good rheological, has reduced organic usage quantity.
4, water-based tape casting trichroite green compact have good release property, and demould time is short, do not need to add the carrier band that tensio-active agent or effects on surface silicon processed and carry out extra process, simplification casting technique process and production cost.
Description of drawings:
Fig. 1 is that example 1 middle shear rate is on the impact of slurry viscosity.
Fig. 2 is cordierite water-based tape casting green compact SEM figure in the example 1.
Embodiment:
Embodiment 1:
A kind of magnesium phase-enriched cordierite water-based tape casting slurry provided by the invention, its component and mass percent are: trichroite 18%, sodium polyacrylate solution 9%, polyvinyl alcohol solution 36.4%, polyglycol solution 8.6%, ultrapure water 28%.The sodium polyacrylate solution concentration 4% of using, the concentration of polyvinyl alcohol solution are 5%, and polyglycol solution concentration is 17%.
The preparation method of a kind of magnesium phase-enriched cordierite water-based tape casting slurry that the present invention proposes may further comprise the steps:
1, be that to join massfraction be in 28% the ultrapure water to 18% cordierite powder with massfraction, glass stick stirs, ultrapure water is in cordierite powder and adds massfraction behind the loose Heshui state is 9% sodium polyacrylate solution, continues to stir into the emulsus slurry.
2, the emulsus slurry in the step 1 is inserted in the zirconia ball grinding jar, take the zirconia ball mill as ball-milling medium, ball milling 6 hours for the first time in planetary comprehensive ball mill obtains elementary slurry.
3, be that 36.4% polyvinyl alcohol solution, massfraction are that 8.6% polyglycol solution joins in the elementary slurry that step 2 obtains with massfraction, ball milling 18 hours for the second time in planetary comprehensive ball mill, obtain cordierite water-based tape casting slurry, solid content is 18%.
4, the cordierite water-based tape casting slurry that the second time, ball milling obtained is placed on the froth in vacuum machine, froth in vacuum is 60 minutes under the room temperature.
5, at room temperature, with the cordierite water-based tape casting slurry sealing and standing after the froth in vacuum 30 minutes, then namely obtain a kind of magnesium phase-enriched cordierite water-based tape casting slurry.
Resulting slurry is that pseudoplastic fluid meets the curtain coating requirement, and the relation of its shearing rate and viscosity as shown in Figure 1; Adopt this slurry curtain coating gained green compact even compact as shown in Figure 2.
Embodiment 2
A kind of magnesium phase-enriched cordierite water-based tape casting slurry provided by the invention, its component and mass percent are: trichroite 35%, sodium polyacrylate solution 18%, polyvinyl alcohol solution 31%, polyglycol solution 6%, ultrapure water 10%.The sodium polyacrylate solution concentration 4% of using, the concentration of polyvinyl alcohol solution are 5%, and polyglycol solution concentration is 17%.
The preparation method of a kind of magnesium phase-enriched cordierite water-based tape casting slurry that the present invention proposes may further comprise the steps:
1, be that to join massfraction be in 15% the ultrapure water to 35% cordierite powder with massfraction, glass stick stirs, ultrapure water is in cordierite powder and adds massfraction behind the loose Heshui state is 18% sodium polyacrylate solution, continues to stir into the emulsus slurry.
2, the emulsus slurry in the step 1 is inserted in the zirconia ball grinding jar, take the zirconia ball mill as ball-milling medium, ball milling 6 hours for the first time in planetary comprehensive ball mill obtains elementary slurry.
3, be that 34.8% polyvinyl alcohol solution, massfraction are that 7.2% polyglycol solution joins in the elementary slurry that step 2 obtains with massfraction, ball milling 17 hours for the second time in planetary comprehensive ball mill, obtain cordierite water-based tape casting slurry, solid content is 35%.
4, the cordierite water-based tape casting slurry that the second time, ball milling obtained is placed on the froth in vacuum machine, froth in vacuum is 50 minutes under the room temperature.
5, at room temperature, with the cordierite water-based tape casting slurry sealing and standing after the froth in vacuum 20 minutes, then namely obtain a kind of magnesium phase-enriched cordierite water-based tape casting slurry.
Embodiment 3
A kind of magnesium phase-enriched cordierite water-based tape casting slurry provided by the invention, its component and mass percent are: trichroite 25%, sodium polyacrylate solution 15%, polyvinyl alcohol solution 32%, polyglycol solution 8%, ultrapure water 20%.The sodium polyacrylate solution concentration 4% of using, the concentration of polyvinyl alcohol solution are 5%, and polyglycol solution concentration is 17%.
The preparation method of a kind of magnesium phase-enriched cordierite water-based tape casting slurry that the present invention proposes may further comprise the steps:
1, be that to join massfraction be in 20% the ultrapure water to 25% cordierite powder with massfraction, glass stick stirs, ultrapure water is in cordierite powder and adds massfraction behind the loose Heshui state is 15% sodium polyacrylate solution, continues to stir into the emulsus slurry.
2, the emulsus slurry in the step 1 is inserted in the zirconia ball grinding jar, take the zirconia ball mill as ball-milling medium, ball milling 6 hours for the first time in planetary comprehensive ball mill obtains elementary slurry.
3, be that 32% polyvinyl alcohol solution, massfraction are that 8% polyglycol solution joins in the elementary slurry that step 2 obtains with massfraction, ball milling 16 hours for the second time in planetary comprehensive ball mill, obtain cordierite water-based tape casting slurry, solid content is 25%.
4, the cordierite water-based tape casting slurry that the second time, ball milling obtained is placed on the froth in vacuum machine, froth in vacuum is 30 minutes under the room temperature.
5, at room temperature, with the cordierite water-based tape casting slurry sealing and standing after the froth in vacuum 15 minutes, then namely obtain a kind of magnesium phase-enriched cordierite water-based tape casting slurry.
Claims (1)
1. the preparation method of a magnesium phase-enriched cordierite water-based tape casting slurry, it is characterized in that: its component and mass percent are: trichroite 15%～35%, sodium polyacrylate solution 8%～18%, polyvinyl alcohol solution 30%～40%, polyglycol solution 5%～10%, ultrapure water 10%～40%; The sodium polyacrylate solution concentration 4% of using, the concentration of polyvinyl alcohol solution are 5%, and polyglycol solution concentration is 17%; Its preparation method may further comprise the steps:
(1), be that to join massfraction be in 10%～40% the ultrapure water to 15%～35% cordierite powder with massfraction, glass stick stirs, ultrapure water is the sodium polyacrylate solution that adds massfraction 8%～18% behind the loose Heshui state in cordierite powder, continue to stir into the emulsus slurry;
(2), the emulsus slurry in the step 1 is inserted in the zirconia ball grinding jar, take the zirconia ball mill as ball-milling medium, ball milling 6 hours for the first time in planetary comprehensive ball mill obtains elementary slurry;
(3), be that 30%～40% polyvinyl alcohol solution, massfraction are that 5%～10% polyglycol solution adds in the elementary slurry that step 2 obtains with massfraction, ball milling 16～18 hours for the second time in planetary comprehensive ball mill, obtain cordierite water-based tape casting slurry, solid content is 15%～35%;
(4), for the second time the cordierite water-based tape casting slurry that obtains of ball milling places on the froth in vacuum machine, froth in vacuum is 30～60 minutes under the room temperature;
(5), at room temperature, with the cordierite water-based tape casting slurry sealing and standing after the froth in vacuum 15～30 minutes, then namely obtain a kind of magnesium phase-enriched cordierite water-based tape casting slurry.
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|---|---|---|---|
| CN 201010209508 CN101870577B (en) | 2010-06-25 | 2010-06-25 | Preparation method of magnesium phase-enriched cordierite water-based tape casting slurry |
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| CN 201010209508 CN101870577B (en) | 2010-06-25 | 2010-06-25 | Preparation method of magnesium phase-enriched cordierite water-based tape casting slurry |
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| CN103351157A (en) * | 2013-06-26 | 2013-10-16 | 沈阳大学 | Technology for controlling sintering shrinkage and deformation of low-temperature co-firing ceramic substrate |
| CN103342550A (en) * | 2013-06-28 | 2013-10-09 | 沈阳大学 | Bonding method based lamination process of cordierite ceramic blank piece |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0423752A3 (en) * | 1989-10-19 | 1992-05-06 | E.I. Du Pont De Nemours And Company | Dielectric compositions |
| CN1534001A (en) * | 2003-04-02 | 2004-10-06 | 珠海粤科清华电子陶瓷有限公司 | Method of preparing zirconium oxide ceramic by curtain coating method and product obtained from said method |
| CN101100390A (en) * | 2007-04-27 | 2008-01-09 | 中国科学院上海硅酸盐研究所 | Method for recasting and reforming molded water-base casting film |
| CN101747025A (en) * | 2009-12-24 | 2010-06-23 | 中国科学院过程工程研究所 | Beta''-Al2O3 solid electrolyte precursor aqueous tape casting slurry and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8607596D0 (en) * | 1986-03-26 | 1986-04-30 | Ici Plc | Dispersible composition of ceramic |
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2010
- 2010-06-25 CN CN 201010209508 patent/CN101870577B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0423752A3 (en) * | 1989-10-19 | 1992-05-06 | E.I. Du Pont De Nemours And Company | Dielectric compositions |
| CN1534001A (en) * | 2003-04-02 | 2004-10-06 | 珠海粤科清华电子陶瓷有限公司 | Method of preparing zirconium oxide ceramic by curtain coating method and product obtained from said method |
| CN101100390A (en) * | 2007-04-27 | 2008-01-09 | 中国科学院上海硅酸盐研究所 | Method for recasting and reforming molded water-base casting film |
| CN101747025A (en) * | 2009-12-24 | 2010-06-23 | 中国科学院过程工程研究所 | Beta''-Al2O3 solid electrolyte precursor aqueous tape casting slurry and preparation method thereof |
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