CN103058665A - Ceramic casting slurry and preparation method thereof - Google Patents
Ceramic casting slurry and preparation method thereof Download PDFInfo
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- CN103058665A CN103058665A CN2011103197944A CN201110319794A CN103058665A CN 103058665 A CN103058665 A CN 103058665A CN 2011103197944 A CN2011103197944 A CN 2011103197944A CN 201110319794 A CN201110319794 A CN 201110319794A CN 103058665 A CN103058665 A CN 103058665A
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Abstract
The invention relates to a ceramic casting slurry and a preparation method thereof. The ceramic casting slurry is characterized by comprising a ceramic powder, a mixed solvent of alcohol and ester, a binder, a plasticizer and a dispersing agent; and the ceramic powder accounts for 65-75wt%, and a weight ratio of the ceramic powder to the mixed solvent is 5:2-4:1. The ceramic casting slurry provided by the invention has high solid content; and the mixed solvent of alcohol and ester has low cost, good environment compatibility, and low poison to the human body.
Description
Technical field
The present invention relates to ceramic thick film curtain coating preparation field, be specifically related to a kind of ceramic casting slurry, especially based on enviroment protective ceramic casting slurry of alcohol-ester mixed solvent and preparation method thereof.
Background technology
The ceramic thick film curtain coating be a kind of have six more than ten years history the ceramic thick film fabricating technology, be the technique basis of multilayerceramic device.Casting method technique generally includes slurry preparation, ball milling, moulding, peel off the process such as base band, but this technique has that equipment is simple, process stabilizing operate continuously, production efficiency advantages of higher, can realize increasingly automated.And the flow casting molding thickness of controlling diaphragm easily, be conducive to the mould material of different components and thickness is designed and structure regulating, to obtain property.In recent years, the application of casting method forming technique makes great progress, and is widely used in the fields such as electronic industry, the energy.
Acquisition material dispersion casting slurry even, modest viscosity is the key of casting method forming technique.Usually, casting slurry is by the ceramic powder of definite composition, proportioning, solvent and organic forming agent (comprising binding agent, dispersion agent and softening agent etc.), successively add according to certain technological process, adopt the method for ball milling, mix within a certain period of time and form.
According to the difference of the solvent that adopts, the casting slurry system mainly comprises two kinds of water-based tape casting and non-aqueous tape-castings.Traditional non-aqueous tape-casting slurry adopts aromatic hydrocarbon such as benzene,toluene,xylene mostly, ketone such as butanone, methylethylketone etc. or its mixture are solvent, to realize the excellent dissolution to caking agent, in drying process, have fast volatilization simultaneously, thereby can obtain high-quality ceramic curtain coating thick film.But toluene, dimethylbenzene equal solvent have higher toxicity, cause environmental pollution after the discharging, are detrimental to health, and these solvent prices, so that corresponding ceramic curtain coating thick film production cost is high.Non-aqueous tape-casting technique, cost is low, pollute less, Environmental compatibility is good, but the influence factor of this technique is many, and because the evaporation rate of water is slow, and the dry difficulty of curtain coating thick film affect ceramic thick film and gives birth to and be with quality.
In recent years, people have carried out many research to the environment-friendly type non-aqueous tape-casting slurry.Low-molecular-weight ester class such as ethyl acetate also are the organic solvents of commonly using, and have with toluene, dimethylbenzene etc. close boiling characteristics is arranged, and can be used to casting slurry has more highly toxic solvent to replace these.Yet casting slurry not only will have the curtain coating thick film of suitable boiling characteristics to obtain with solvent, and also needing in addition has good solvability to used caking agent.At present, often adopt polyvinyl butyral acetal (PVB) as binding agent at the preparation casting slurry, and low-molecular-weight ester class such as ethyl acetate is dissolved binding agent such as polyvinyl formal etc. in the mode of swelling, solubleness is relatively low, far below toluene.Therefore, in the situation of same solvent consumption, the viscosity of the slurry take the ester class as solvent is larger, can't obtain high-quality curtain coating thick film; And to obtain identical viscosities, and then to strengthen solvent load, cause the slurry solid content to reduce.
Alcoholic solvent has good solvability to ceramic bonding agent such as polyvinyl formal.CN 102093577 A disclose a kind of environmentally friendly solvent, and it comprises ester class and alcohols.Intrinsic understanding in view of those skilled in the art, the volatility of alcoholic solvent is lower and polarity is all unfavorable to obtaining high-quality curtain coating thick film more by force, therefore, and in the disclosed scheme of CN 102093577 A, as main solvent, and just add alcohols as solubility promoter with the ester class of low volatility.In the disclosed scheme of CN 102093577 A, increased solvability to binding agent although added alcohols as solubility promoter, yet solid load is still lower in the disclosed casting slurry of this scheme, its disclosed 3 embodiments, with the powder content of embodiment one for the highest (about 56 wt%), and the total solvent amount of corresponding employing is still larger, and the weight ratio of powder and solvent for use is about 2:1 to the maximum.Therefore, need the relatively few alcohol of further research solid load height and solvent load-ester group casting slurry, with for the preparation of the high thick film ceramic material of performance.
Summary of the invention
The problems referred to above in the face of the prior art existence, the invention provides a kind of new ceramics casting slurry, the mixed solvent, binding agent, softening agent and the dispersion agent that comprise ceramic powder, pure and mild ester, wherein, the weight percentage of described ceramic powder can be 65～75 wt%, and the weight ratio of described ceramic powder and mixed solvent can be 5:2～4:1.
As solvent, the cost check and correction is lower with alcohol-ester mixed solvent for ceramic casting slurry provided by the invention, and Environmental compatibility is good, and is lower to the human body toxic.Adopt alcohol-ester mixed solvent can regulate solvent and make its evaporation rate near traditional toluene, dimethylbenzene evaporation rate, be beneficial to casting technique control.And mixed solvent has good solubility to binding agent, thereby can obtain the casting slurry that viscosity is low and solid load is high, ceramic casting slurry of the present invention for example, ceramic powder content is up to 65～75 wt%, and the weight ratio of itself and solvent for use can be up to 4:1, and solid load is high, the solvent for use amount is little, be particularly suitable for casting method and prepare the thick film ceramic material, for example can prepare tens microns even millimetre-sized ceramic green band, have broad application prospects.
In the present invention, the weight percentage of alcohol can be 20～70 wt%, preferred 40～60 wt% in the described mixed solvent.The content of alcohol is higher in the used mixed solvent of the present invention, and is good to the solvability of binding agent, is conducive to improve in the slurry solid load and can reduces viscosity, is conducive to flow casting molding.
In the present invention, the alcohol in the described mixed solvent can be a kind of or any several mixture in ethanol, propyl alcohol, Virahol, ethylene glycol, propyl carbinol, isopropylcarbinol, the trimethyl carbinol, phenylethyl alcohol, the diacetone alcohol; Ester in the described mixed solvent can be one or more the mixture in methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butylacetate, the isobutyl acetate.Pure and mild ester in the used mixed solvent of the present invention, the source is abundant, and is cheap and easy to get, reduced production cost.
In the present invention, the weight percentage of described binding agent and softening agent can be 4～8 wt%.Wherein, the weight ratio of described binding agent and softening agent can be 3:2～4:1.Described binding agent can be polyvinyl butyral acetal.Described softening agent can be the mixture of phthalic ester and polyoxyethylene glycol.Wherein the weight ratio of phthalic ester and polyoxyethylene glycol can be 1:3～3:1.
On the other hand, the present invention also provides a kind of method for preparing above-mentioned ceramic casting slurry, comprising: dispersion agent, described ceramic powder are added part or all of described mixed solvent carry out ball milling one time; Then add described binding agent or described binding agent and be dissolved in the binder solution of the formation of the described mixed solvent of part, and softening agent carries out secondary ball milling, obtain described ceramic casting slurry.
In the present invention, a described Ball-milling Time can be 8～12 hours, and for example 10 hours, the described secondary ball milling time can be 36～50 hours, for example 48 hours.
Preparation method's raw material of the present invention is simple, cost is low and technical process is simple, and controllability is high, good reproducibility, and Environmental compatibility is good, is fit to scale production.The casting slurry solid load of method preparation of the present invention is high, is suitable for preparing ceramic thick film material flow casting molding, and the curtain coating preparation of electronic ceramics thick films such as ceramic dielectric, piezoelectric ceramics, LTCC has fabulous application prospect.
Embodiment
Further specify the present invention with reference to following embodiment, should be understood that following embodiment only is used for explanation the present invention, and unrestricted the present invention.
Two step of the employing ball milled preparation of the present invention's pottery casting slurry.
1) ceramic powder, all or part of mixed solvent, dispersion agent are joined ball grinder, grind (ball milling) at ball mill, so that ceramic powder fully disperses.
2) binding agent or binding agent are dissolved in the binder solution of the formation of partially mixed solvent, and softening agent adds in the mixture of dispersion of step 1) gained, continue ball milling (secondary ball milling), obtain ceramic casting slurry.In the present invention, one time Ball-milling Time can be 8～12 hours, and for example 10 hours, the secondary ball milling time can be 36～50 hours, for example 48 hours.
Ceramic powder in the present invention's pottery casting slurry includes but not limited to ceramic dielectric, piezoelectric ceramics, LTCC, used ceramic powder particle diameter can be 0.1～10 micron, for example adopts commercially available X7R dielectric ceramic powder or self-control low-k LTCC (diameter of particle is 0.5～3 micron).In the present invention's pottery casting slurry, the weight percent of ceramic powder can reach 65～75 wt%, and solid load is high.
Mixed solvent in the present invention's pottery casting slurry can be comprised of alcohols and ester class, alcohols can be one or more the mixture in ethanol, propyl alcohol, Virahol, ethylene glycol, propyl carbinol, isopropylcarbinol, the trimethyl carbinol, phenylethyl alcohol, the diacetone alcohol, the ester class is one or more the mixture in methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butylacetate, the isobutyl acetate, the content of alcohol can be 20～70 wt%, preferred 40～60 wt% in the mixed solvent.In the present invention pottery casting slurry, solvent load is relatively less, and the weight ratio of itself and ceramic powder can 1:4～2:5.The Viscosity of Slurry for Tape casting that forms like this is lower, volatilization is very fast.
Dispersion agent in the present invention pottery casting slurry can be a kind of in nonpolar dispersion agent, amphoteric dispersant, anionic dispersing agent and the cationic dispersing agent, for example triglyceride, tributyl phosphate.
Caking agent in the present invention's pottery casting slurry can be polyvinyl butyral acetal, and its polymerization degree can be 400-1000, and hydroxy radical content can be 10～25%.Softening agent can be phthalic ester, polyoxyethylene glycol or both mixtures.Wherein phthalic ester is at least a in dioctyl phthalate (DOP), phthalic acid two (2-ethylhexyl) ester, dibutyl phthalate, butyl benzyl phthalate, diethyl phthalate, dipropyl phthalate, the diisobutyl phthalate.The polyethylene glycol polymeric degree can be 200～800.In the softening agent by phthalic ester and polyoxyethylene glycol compositions of mixtures, the mass ratio of phthalic ester and polyoxyethylene glycol is 1:3～3:1, preferred 1:1.In the present invention's pottery casting slurry, the gross weight percentage composition of caking agent and softening agent can be 4～8 wt%, and the mass ratio of caking agent and softening agent can be 3:2～4:1.
The alcohol of the present invention's pottery casting slurry employing environment-friendly type-ester mixed solvent, mixed solvent has good solubility to the ceramic bonding agent, makes ceramic casting slurry that high solid content be arranged thereby can obtain low viscosity; Adopt alcohol-ester mixed solvent can regulate solvent evaporates speed and make it to approach with traditional toluene, xylene solvent evaporation rate, be beneficial to casting technique control; On the other hand, alcohols and ester class price are relatively cheap, are easy to promote.Then the casting slurry of present method preparation can curtain coating go out tens microns to hundreds of micron thickness even millimetre-sized ceramic green band on full-automatic casting machine, ceramic green band and pet vector film are wetting good, it is high to give birth to band density, for example can reach 3.5 g/ccs, has good snappiness.
The present invention further illustrates following embodiment so that the present invention to be described better.
Embodiment 1:
Mixed solvent consist of dehydrated alcohol and ethyl acetate, both weight ratios are 1:1.Caking agent is the polyvinyl formal B06SY of Changchun, Taiwan petroleum chemistry company, and caking agent is dissolved in above-mentioned mixed solvent, obtains the solution of 30 wt%, and the consumption of adhesive solution is 80 grams.Ceramic powder is the X7R dielectric ceramic powder, and consumption is 500 grams.Solvent load is 105 grams.Dispersion agent is triglyceride, and consumption is 1.5 wt% of ceramic powder.Softening agent is butyl benzyl phthalate and poly(oxyethylene glycol) 400, and both ratios are 1:1, and the total consumption of softening agent is 50 wt% of caking agent.First ceramic powder, solvent and dispersion agent are added the nylon ball grinder ball milling 10 hours during the preparation slurry, then above-mentioned adhesive solution and softening agent are joined ball grinder continuation ball milling 48 hours, obtain casting slurry.The casting slurry of present method preparation curtain coating on full-automatic casting machine goes out the ceramic green band of 30 micron thickness, and ceramic green band and pet vector film are wetting good, gives birth to band density and reaches 3.5 g/ccs, has good snappiness.
The step that repeats embodiment 1 by the proportioning of following table 1 prepares the ceramic casting slurry of following embodiment:
Table 1:
In the above-described embodiments, although ethanol, Virahol, ethylene glycol, isopropylcarbinol only are shown as the example alcohols, take ethyl acetate, ethyl acetate, isopropyl acetate as example ester class, but should understand, the alcohols that other are suitable and ester class also are suitable for, also can be a kind of in propyl alcohol, Virahol, propyl carbinol, the trimethyl carbinol, phenylethyl alcohol, the diacetone alcohol etc. or any several mixture such as alcohols, the ester class also can be one or more the mixture in methyl acetate, butylacetate, the isobutyl acetate etc.Powder can adopt ceramic dielectric commonly used, piezoelectric ceramics, LTCC as required, used ceramic powder particle diameter can be 0.1～10 micron, for example adopts commercially available X7R dielectric ceramic powder or self-control low-k LTCC (diameter of particle is 0.5～3 micron).Dispersion agent can be a kind of in nonpolar dispersion agent, amphoteric dispersant, anionic dispersing agent and the cationic dispersing agent, for example triglyceride, tributyl phosphate.Caking agent can be polyvinyl butyral acetal, and its polymerization degree can be 400-1000, and hydroxy radical content can be 10～25%.Softening agent can be phthalic ester, polyoxyethylene glycol or both mixtures.Wherein phthalic ester is at least a in dioctyl phthalate (DOP), phthalic acid two (2-ethylhexyl) ester, dibutyl phthalate, butyl benzyl phthalate, diethyl phthalate, dipropyl phthalate, the diisobutyl phthalate.The polyethylene glycol polymeric degree can be 200～800.In the softening agent by phthalic ester and polyoxyethylene glycol compositions of mixtures, the mass ratio of phthalic ester and polyoxyethylene glycol is 1:3～3:1, preferred 1:1.
Industrial applicability: casting slurry of the present invention adopts pure and mild ester mixed solvent cheap and easy to get, that toxicity is relatively low, cost is low, Environmental compatibility good.And casting slurry solid load of the present invention is high, and solvent load is relatively few, is particularly suitable for casting method and prepares the thick film ceramic material, for example can prepare tens microns even millimetre-sized ceramic green band, has broad application prospects.Preparation method's raw material of the present invention is simple, cost is low and technical process is simple, and controllability is high, good reproducibility, and Environmental compatibility is good, is fit to scale production.
Claims (10)
1. ceramic casting slurry, it is characterized in that, described ceramic casting slurry comprises mixed solvent, binding agent, softening agent and the dispersion agent of ceramic powder, pure and mild ester, wherein, the weight percentage of described ceramic powder is 65～75 wt%, and the weight ratio of described ceramic powder and mixed solvent is 5:2～4:1.
2. ceramic casting slurry according to claim 1 is characterized in that, the weight percentage of alcohol is 20～70 wt% in the described mixed solvent.
3. ceramic casting slurry according to claim 2 is characterized in that, the weight percentage of alcohol is 40～60 wt% in the described mixed solvent.
4. each described ceramic casting slurry in 3 according to claim 1, it is characterized in that the alcohol in the described mixed solvent is a kind of or any several mixture in ethanol, propyl alcohol, Virahol, ethylene glycol, propyl carbinol, isopropylcarbinol, the trimethyl carbinol, phenylethyl alcohol, the diacetone alcohol; Ester in the described mixed solvent is one or more the mixture in methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butylacetate, the isobutyl acetate.
5. ceramic casting slurry according to claim 1 is characterized in that, the gross weight percentage composition of described binding agent and softening agent is 4～8 wt%.
6. ceramic casting slurry according to claim 5 is characterized in that, described binding agent is polyvinyl butyral acetal, and described softening agent is the mixture of phthalic ester and polyoxyethylene glycol.
7. ceramic casting slurry according to claim 6 is characterized in that, in described softening agent, the weight ratio of phthalic ester and polyoxyethylene glycol is 1:3～3:1.
8. each described ceramic casting slurry in 7 according to claim 5 is characterized in that the weight ratio of described binding agent and softening agent is 3:2～4:1.
9. a method for preparing ceramic casting slurry claimed in claim 1 is characterized in that, comprising:
Dispersion agent, described ceramic powder are added part or all of described mixed solvent carry out ball milling one time;
Then add described binding agent or described binding agent and be dissolved in the binder solution of the formation of the described mixed solvent of part, and softening agent carries out secondary ball milling, obtain described ceramic casting slurry.
10. method according to claim 9 is characterized in that, a described Ball-milling Time is 8～12 hours, and the described secondary ball milling time is 36～50 hours.
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Cited By (14)
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| CN103435358A (en) * | 2013-08-29 | 2013-12-11 | 中国人民解放军国防科学技术大学 | Organic composition added in preparation of tape-casting slurry and application of organic composition |
| CN104045352A (en) * | 2014-05-28 | 2014-09-17 | 镇江博威汽车科技有限公司 | Dispersant for preparing zirconia tape-casted sheet and application thereof |
| CN104261808A (en) * | 2014-09-09 | 2015-01-07 | 登封福中特种电器元件有限公司 | High-temperature conductor paste for printing electronic ceramic cast slice |
| CN104261809A (en) * | 2014-09-09 | 2015-01-07 | 登封福中特种电器元件有限公司 | Processing method of electronic ceramic tape-casting slurry |
| CN106830948A (en) * | 2016-11-14 | 2017-06-13 | 中国科学院上海硅酸盐研究所 | Ceramic casting slurry based on poly (propylene carbonate) binding agent and its preparation method and application |
| CN107235714A (en) * | 2017-08-01 | 2017-10-10 | 郑州联冠科技有限公司 | Electronic ceramics casting slurry configuration technique |
| CN107805074A (en) * | 2017-11-13 | 2018-03-16 | 戴承萍 | A kind of processing method of electronic ceramics casting slurry |
| CN110483044A (en) * | 2019-09-25 | 2019-11-22 | 哈尔滨工业大学 | A kind of high-Q microwave dielectric ceramics and aluminium ultralow temperature co-burning method and high-Q microwave dielectric ceramic preparation |
| CN113698212A (en) * | 2021-08-18 | 2021-11-26 | 江苏富乐德半导体科技有限公司 | Ceramic tape-casting slurry and preparation method thereof |
| CN113716951A (en) * | 2021-08-26 | 2021-11-30 | 新沂市锡沂高新材料产业技术研究院有限公司 | Preparation method of YAG-based transparent ceramic with large-size sheet composite structure |
| CN114538900A (en) * | 2022-02-16 | 2022-05-27 | 中国科学院上海硅酸盐研究所 | High-purity ultrathin high-strength alumina ceramic substrate and preparation method and application thereof |
| CN114560683A (en) * | 2022-02-16 | 2022-05-31 | 中国科学院上海硅酸盐研究所 | Environment-friendly low-toxicity ceramic tape-casting slurry and preparation method and application thereof |
| CN114933476A (en) * | 2022-06-10 | 2022-08-23 | 北京智感度衡科技有限公司 | Zirconia green ceramic chip for nitrogen-oxygen sensor and preparation method thereof |
| CN115974531A (en) * | 2023-02-16 | 2023-04-18 | 浙江矽瓷科技有限公司 | Low-temperature co-fired ceramic tape-casting slurry and preparation method thereof |
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| CN103435358A (en) * | 2013-08-29 | 2013-12-11 | 中国人民解放军国防科学技术大学 | Organic composition added in preparation of tape-casting slurry and application of organic composition |
| CN103435358B (en) * | 2013-08-29 | 2015-03-25 | 中国人民解放军国防科学技术大学 | Organic composition added in preparation of tape-casting slurry and application of organic composition |
| CN104045352A (en) * | 2014-05-28 | 2014-09-17 | 镇江博威汽车科技有限公司 | Dispersant for preparing zirconia tape-casted sheet and application thereof |
| CN104045352B (en) * | 2014-05-28 | 2015-08-05 | 镇江博威汽车科技有限公司 | A kind of dispersion agent for the preparation of zirconium white cast sheet and application thereof |
| CN104261808A (en) * | 2014-09-09 | 2015-01-07 | 登封福中特种电器元件有限公司 | High-temperature conductor paste for printing electronic ceramic cast slice |
| CN104261809A (en) * | 2014-09-09 | 2015-01-07 | 登封福中特种电器元件有限公司 | Processing method of electronic ceramic tape-casting slurry |
| CN106830948A (en) * | 2016-11-14 | 2017-06-13 | 中国科学院上海硅酸盐研究所 | Ceramic casting slurry based on poly (propylene carbonate) binding agent and its preparation method and application |
| CN107235714A (en) * | 2017-08-01 | 2017-10-10 | 郑州联冠科技有限公司 | Electronic ceramics casting slurry configuration technique |
| CN107805074A (en) * | 2017-11-13 | 2018-03-16 | 戴承萍 | A kind of processing method of electronic ceramics casting slurry |
| CN110483044A (en) * | 2019-09-25 | 2019-11-22 | 哈尔滨工业大学 | A kind of high-Q microwave dielectric ceramics and aluminium ultralow temperature co-burning method and high-Q microwave dielectric ceramic preparation |
| CN110483044B (en) * | 2019-09-25 | 2021-08-13 | 哈尔滨工业大学 | high-Q-value microwave dielectric ceramic and aluminum ultralow-temperature co-firing method and high-Q-value microwave dielectric ceramic preparation method |
| CN113698212A (en) * | 2021-08-18 | 2021-11-26 | 江苏富乐德半导体科技有限公司 | Ceramic tape-casting slurry and preparation method thereof |
| CN113716951A (en) * | 2021-08-26 | 2021-11-30 | 新沂市锡沂高新材料产业技术研究院有限公司 | Preparation method of YAG-based transparent ceramic with large-size sheet composite structure |
| CN113716951B (en) * | 2021-08-26 | 2022-04-29 | 新沂市锡沂高新材料产业技术研究院有限公司 | Preparation method of YAG-based transparent ceramic with large-size sheet composite structure |
| CN114538900A (en) * | 2022-02-16 | 2022-05-27 | 中国科学院上海硅酸盐研究所 | High-purity ultrathin high-strength alumina ceramic substrate and preparation method and application thereof |
| CN114560683A (en) * | 2022-02-16 | 2022-05-31 | 中国科学院上海硅酸盐研究所 | Environment-friendly low-toxicity ceramic tape-casting slurry and preparation method and application thereof |
| CN114933476A (en) * | 2022-06-10 | 2022-08-23 | 北京智感度衡科技有限公司 | Zirconia green ceramic chip for nitrogen-oxygen sensor and preparation method thereof |
| CN115974531A (en) * | 2023-02-16 | 2023-04-18 | 浙江矽瓷科技有限公司 | Low-temperature co-fired ceramic tape-casting slurry and preparation method thereof |
| CN115974531B (en) * | 2023-02-16 | 2023-12-26 | 浙江矽瓷科技有限公司 | Low-temperature cofired ceramic tape casting slurry and preparation method thereof |
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Application publication date: 20130424 |