CN103056958A - Method for preparing piezoelectric ceramic piece green compact by using aqueous tape casting - Google Patents
Method for preparing piezoelectric ceramic piece green compact by using aqueous tape casting Download PDFInfo
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- CN103056958A CN103056958A CN2012105882273A CN201210588227A CN103056958A CN 103056958 A CN103056958 A CN 103056958A CN 2012105882273 A CN2012105882273 A CN 2012105882273A CN 201210588227 A CN201210588227 A CN 201210588227A CN 103056958 A CN103056958 A CN 103056958A
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Abstract
The invention discloses a method for preparing piezoelectric ceramic piece green compact by using aqueous tape casting and belongs to methods for preparing piezoelectric ceramic piece green compact. The method includes the steps of: (1) adding n-caprylic alcohol into tape casting slurry and vacuumizing to achieve deaeration and (2) drying the deaired tape casting slurry by using a tape casting machine in a tape casting mode. The tape casting slurry is prepared from, by weight percentage, 60-70 percent of piezoelectric ceramic powder, 3-13 percent of acrylic resin emulsion, 0.1-2 percent of dispersing agent, 0.1-0.3 percent dioctyl phthalate and the remaining percent of deionized water. The preparation method includes the steps of: (1) mixing the piezoelectric ceramic powder with dispersing agent aqueous solution evenly and ball-milling to obtain ceramic slurry, (2) adding the acrylic resin emulsion and the dioctyl phthalate into the ceramic slurry and ball-milling to obtain the tape casting slurry. According to the method for preparing piezoelectric ceramic piece green compact by using aqueous tape casting, the surface tension of the tape casting slurry is close to the surface tension of steel strips so that the good moistening effect is achieved.
Description
Technical field
The present invention relates to a kind of method of utilizing the tape casting to prepare the piezoelectric ceramic piece green compact, relate in particular to a kind ofly take water as solvent, adopt the tape casting to prepare the method for piezoelectric ceramic piece green compact.
Background technology:Curtain coating is one of technique of preparation piezoelectric ceramics diaphragm material, and it is divided into water-based tape casting and non-aqueous tape-casting.Non-aqueous tape-casting technique comparative maturity, the diaphragm of preparation is homogeneous, intensity is high, good toughness, be convenient to cutting and processing, uses in actual production for many years; But non-aqueous tape-casting technique need use a large amount of poisonous organic matters as solvent, and not only production cost is high, and easily causes environmental pollution.As solvent, the organic matter consumption is few, cost is low with water for water-based flow casting technique, it is little to pollute, and the Environmental compatibility industry is good.Yet now widely used casting apparatus generally adopts the casting films band of steel, and this film band mainly is to design for non-aqueous tape-casting technique, and its surface tension is usually about 19 dyne; And the aqueous casting slurry surface tension is higher, and is very poor to the wetability of steel casting films belt surface; Can occur before forming tape casting diaphragm very significantly shrinking at slurry drying, therefore the designing requirement that does not reach piezoelectric ceramic piece need to prolong technique to base flow and improve.
Summary of the invention:In view of the foregoing defects the prior art has, the present invention aims to provide the method that a kind of water base casting process prepares the piezoelectric ceramic piece green compact, and the method can be utilized existing flow casting molding machine, adopt water-based flow casting technique to prepare qualified piezoelectric ceramic piece green compact.
To achieve these goals, the technical solution used in the present invention comprises carries out de-bubble processing and curtain coating oven dry to casting slurry, described casting slurry is formulated by the raw material of following percentage by weight: the dispersant 0.1～2% that the meta particle diameter is that 1 micron piezoelectric ceramic powder 60～70%, aggregation degree is 1200～2000, alcoholysis degree is 50～99% emulsion acrylic resin 3～13%, model is D-3019, dioctyl phthalate 0.1～3%, all the other are deionized water, and its method is as follows:
1) will mix in above-mentioned dispersant and the deionized water, then add piezoelectric ceramic powder, ball milling 12～36 hours gets ceramic size;
2) add described emulsion acrylic resin and dioctyl phthalate in above-mentioned ceramic size, ball milling 12～36 hours gets casting slurry;
3) add n-octyl alcohol in the above-mentioned casting slurry and mix, vacuumize de-bubble; The addition of n-octyl alcohol is 0.03～2% of casting slurry volume;
4) with the flow casting molding machine casting slurry of processing through de-bubble is carried out the curtain coating oven dry, get the piezoelectric ceramic piece green compact; The temperature province of this steel band casting machine is 50 ℃, 70 ℃, 90 ℃, 120 ℃, and the curtain coating time is 3～18 minutes.
In technique scheme, emulsion acrylic resin is the stable suspension of acrylic resin polymer, is to carry out emulsion polymerisation by acrylic monomers in water to obtain, and the particle diameter of polymer beads is between 30～500nm.Its advantage is solid content high (concentration can reach 50wt%), viscosity is low, glass transition temperature is low, have certain divergent function, therefore is a kind of binding agent that is fit to very much the preparation casting slurry.Though emulsion acrylic resin is the binding agent of a kind of low viscosity, high solids content, the viscosity of casting slurry is linear growth with the increase of emulsion acrylic resin consumption, therefore must strict control.This is because it is macromolecular compound, molecular chain length, and intermolecular mutual winding makes system viscosity increase easily; Therefore, under the prerequisite that guarantees ceramic green diaphragm intensity, should reduce use amount as far as possible.This not only can increase the density of solid of green compact diaphragm but also can reduce manufacturing cost.
The effect of dispersant is to prevent that ceramic particle from flocculation occuring and cause particles settling, so dispersant is also referred to as " deflocculant ".Its dominant mechanism is to have utilized space steric effect and the Coulomb repulsion effect of dispersant molecule, therefore can significantly increase the repulsive interaction between the PZT powder particle.Under the certain condition of solid content, can obviously reduce the viscosity (when not using dispersant, slurry viscosity is 250cP, and when dispersant dosage was 0.4 wt%, viscosity was dropped rapidly to 120cP) of slurry.Yet when dispersant dosage was much, slurry viscosity increased on the contrary to some extent.This is that unnecessary dispersant can only be dissolved in the solvent because when dispersant dosage surpassed finite concentration, the ceramic powder particle surface was dispersed agent molecule fully and wraps up.And dispersant is macromolecular compound, has backbone, and the interaction between them will cause the increase of slurry viscosity.As seen dispersant dosage is not to be the bigger the better, but has optimum amount.
Usually, in order to reduce the required heat of evaporating solvent, improve diaphragm intensity, to increase efficient, often wish that slurry has higher solid content; Can reduce so organic content and density in the green compact diaphragm.But in the certain situation of other condition, slurry viscosity increases with the increase of solid content, therefore must select suitable range of solid content, avoids slurry viscosity too high.
Compared with the prior art, adopt the present invention owing to adopted technique scheme, with emulsion acrylic resin as binding agent, take dioctyl phthalate as plasticizer and adopt n-octyl alcohol as defrother, cooperate model as the D-3019 dispersant again; Therefore can reduce by the double action of binding agent and plasticizer the surface tension of casting slurry, make its surface tension near steel band (350～600mPa.s), thus reach the purpose of good wet.Adopt the aqueous casting slurry solid content of the inventive method preparation high, its production efficiency exceeds about 50% than PVA system.
The specific embodiment:The invention will be further described below in conjunction with specific embodiment, and concrete steps are as follows:
Embodiment 1
1) take by weighing respectively pressure meta particle diameter and be 1 micron 13 kilograms of 60 kilograms of piezoelectric ceramic powders, emulsion acrylic resins, 3 kilograms of 0.1 kilogram of dispersant, dioctyl phthalates, 23.9 kilograms of the deionized waters that model is D-3019, for subsequent use;
2) above-mentioned dispersant and deionized water are mixed, then add piezoelectric ceramic powder, ball milling 12 hours gets ceramic size;
3) add described emulsion acrylic resin and dioctyl phthalate in above-mentioned ceramic size, ball milling 36 hours gets casting slurry;
4) add n-octyl alcohol in the above-mentioned casting slurry and mix, vacuumize according to a conventional method de-bubble; The addition of n-octyl alcohol is 0.03% of casting slurry volume;
5) according to a conventional method the casting slurry of processing through de-bubble is carried out the curtain coating oven dry with the flow casting molding machine, get the piezoelectric ceramic piece green compact; The temperature province of this steel band casting machine is 50 ℃, 70 ℃, 90 ℃, 120 ℃, and the curtain coating time is 10 minutes.
Embodiment 2
Each step is with embodiment 1; Wherein, piezoelectric ceramic powder in the step 1) is that 70 kilograms, emulsion acrylic resin are that 3 kilograms, dispersant are that 2 kilograms, dioctyl phthalate are 24.9 kilograms of 0.1 kilograms, deionized water, step 2) and the Ball-milling Time in the step 3) be 24 hours, the addition of n-octyl alcohol is 2% of casting slurry volume in the step 4).
Embodiment 3
Each step is with embodiment 1; Wherein, piezoelectric ceramic powder in the step 1) is that 60 kilograms, emulsion acrylic resin are that 3 kilograms, dispersant are that 0.1 kilogram, dioctyl phthalate are 36.8 kilograms of 0.1 kilograms, deionized water, step 2) and the Ball-milling Time in the step 3) be 12 hours, the addition of n-octyl alcohol is 0.03% of casting slurry volume in the step 4), and the curtain coating time in the step 5) is 18 minutes.
Embodiment 4
Each step is with embodiment 1; Wherein, piezoelectric ceramic powder in the step 1) is that 70 kilograms, emulsion acrylic resin are that 13 kilograms, dispersant are that 2 kilograms, dioctyl phthalate are 12 kilograms of 3 kilograms, deionized water, step 2) and the Ball-milling Time in the step 3) be 36 hours, the addition of n-octyl alcohol is 2% of casting slurry volume in the step 4), and the curtain coating time in the step 5) is 3 minutes.
Embodiment 5
Each step is with embodiment 1; Wherein, piezoelectric ceramic powder in the step 1) is that 65 kilograms, emulsion acrylic resin are that 8 kilograms, dispersant are that 1 kilogram, dioctyl phthalate are 24.5 kilograms of 1.5 kilograms, deionized water, step 2) and the Ball-milling Time in the step 3) be 24 hours, the addition of n-octyl alcohol is 1% of casting slurry volume in the step 4), and the curtain coating time in the step 5) is 10 minutes.
In the various embodiments described above, the aggregation degree of emulsion acrylic resin is 1200～2000, alcoholysis degree is 50～99%.
Claims (1)
1. a water base casting process prepares the method for piezoelectric ceramic piece green compact, comprise casting slurry is carried out de-bubble processing and curtain coating oven dry, it is characterized in that described casting slurry is formulated by the raw material of following percentage by weight: the dispersant 0.1～2% that the meta particle diameter is that 1 micron piezoelectric ceramic powder 60～70%, aggregation degree is 1200～2000, alcoholysis degree is 50～99% emulsion acrylic resin 3～13%, model is D-3019, dioctyl phthalate 0.1～3%, all the other are deionized water, and its method is as follows:
1) will mix in above-mentioned dispersant and the deionized water, then add piezoelectric ceramic powder, ball milling 12～36 hours gets ceramic size;
2) add described emulsion acrylic resin and dioctyl phthalate in above-mentioned ceramic size, ball milling 12～36 hours gets casting slurry;
3) add n-octyl alcohol in the above-mentioned casting slurry and mix, vacuumize de-bubble; The addition of n-octyl alcohol is 0.03～2% of casting slurry volume;
4) with the flow casting molding machine casting slurry of processing through de-bubble is carried out the curtain coating oven dry, get the piezoelectric ceramic piece green compact; The temperature province of this steel band casting machine is 50 ℃, 70 ℃, 90 ℃, 120 ℃, and the curtain coating time is 3～18 minutes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115838284A (en) * | 2022-10-08 | 2023-03-24 | 浙江百岸科技有限公司 | Preparation method of water-based casting film belt for nitrogen-oxygen sensor |
| CN113773091B (en) * | 2021-08-11 | 2023-10-24 | 臻金新材(深圳)有限公司 | Aluminum nitride ceramic casting slurry, aluminum nitride ceramic substrate and preparation method |
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| US4751013A (en) * | 1984-08-16 | 1988-06-14 | Siemens Aktiengesellschaft | Porous piezoelectric material and method for making it |
| CN1390807A (en) * | 2002-07-17 | 2003-01-15 | 清华大学 | Process for preparing ceramic sheet from emulsoid system by water-base doctor blading method |
| CN1502586A (en) * | 2002-11-26 | 2004-06-09 | 北京航空材料研究院 | Water-based gel casting forming method for thin ceramic blank sheet |
| JP2005022909A (en) * | 2003-06-30 | 2005-01-27 | Kyocera Corp | Green sheet, its producing method, multilayer piezoelectric body, piezoelectric actuator, and inkjet recording head |
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| CN1911859A (en) * | 2005-08-09 | 2007-02-14 | 黄荣厦 | Curtain casting preparation method of ceramic film sheet for electronic device |
| CN101092299A (en) * | 2007-05-16 | 2007-12-26 | 中材高新材料股份有限公司 | Ceramics powder material of absorbing laser and preparation method |
| CN101328068A (en) * | 2008-07-28 | 2008-12-24 | 浙江大学 | Preparation of boric microwave dielectric ceramic aqueous tape casting diaphragm |
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2012
- 2012-12-29 CN CN2012105882273A patent/CN103056958A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4751013A (en) * | 1984-08-16 | 1988-06-14 | Siemens Aktiengesellschaft | Porous piezoelectric material and method for making it |
| CN1390807A (en) * | 2002-07-17 | 2003-01-15 | 清华大学 | Process for preparing ceramic sheet from emulsoid system by water-base doctor blading method |
| CN1502586A (en) * | 2002-11-26 | 2004-06-09 | 北京航空材料研究院 | Water-based gel casting forming method for thin ceramic blank sheet |
| JP2005022909A (en) * | 2003-06-30 | 2005-01-27 | Kyocera Corp | Green sheet, its producing method, multilayer piezoelectric body, piezoelectric actuator, and inkjet recording head |
| CN1911859A (en) * | 2005-08-09 | 2007-02-14 | 黄荣厦 | Curtain casting preparation method of ceramic film sheet for electronic device |
| CN1803709A (en) * | 2005-12-27 | 2006-07-19 | 中国科学院上海硅酸盐研究所 | Nanometer bismuth titanate aqueous casting slurry and preparation method thereof |
| CN101092299A (en) * | 2007-05-16 | 2007-12-26 | 中材高新材料股份有限公司 | Ceramics powder material of absorbing laser and preparation method |
| CN101328068A (en) * | 2008-07-28 | 2008-12-24 | 浙江大学 | Preparation of boric microwave dielectric ceramic aqueous tape casting diaphragm |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113773091B (en) * | 2021-08-11 | 2023-10-24 | 臻金新材(深圳)有限公司 | Aluminum nitride ceramic casting slurry, aluminum nitride ceramic substrate and preparation method |
| CN115838284A (en) * | 2022-10-08 | 2023-03-24 | 浙江百岸科技有限公司 | Preparation method of water-based casting film belt for nitrogen-oxygen sensor |
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Application publication date: 20130424 |