CN103360060B - Sodium bismuth titanate based textured piezoelectric ceramic water-based tape casting slurry and preparation method of ceramic membrane thereof - Google Patents
Sodium bismuth titanate based textured piezoelectric ceramic water-based tape casting slurry and preparation method of ceramic membrane thereof Download PDFInfo
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Abstract
The invention discloses a sodium bismuth titanate based textured piezoelectric ceramic water-based tape casting slurry, which comprises: 32-69wt% of a ceramic base material, 1-20wt% of a template, 15-55wt% of deionized water, 0.5-5wt% of a dispersant, 5-35wt% of a binder, 1-10wt% of a plasticizer, 0.01-3wt% of a film-forming agent, and 0.02-1wt% of a defoaming agent. The ceramic base material is sodium bismuth titanate based ceramic powder containing 1-5wt% of a sintering additive. The template is sheet Na0.5Bi4.5Ti4O15. In addition, the invention also discloses a method for preparing the ceramic membrane from the slurry. The method disclosed in the invention adopts non-toxic and environment-friendly deionized water as a solvent, thus not only improving the product quality, but also well adapting to the development trends of environment-friendliness and clean production. Also, the process has the advantages of simplicity, low cost and safe use, thus being suitable for large-scale industrial production.
Description
Technical field
The present invention relates to ceramic material technical field, relate in particular to the preparation method of a kind of bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry and ceramic diaphragm thereof.
Background technology
Piezoelectric, as the class sensitization functional material about electricity, power, heat, light, is the important materials of information age, has been widely used in laser, information, navigation, unicircuit, marine charting, has automatically controlled and the field such as biological.In current piezoelectric ceramics field, Pb-based lanthanumdoped zirconate titanates (Pb (Ti, Zr) O
3, be called for short PZT) base pottery be basisization research and practical aspect the most successful piezoelectric ceramics all.But the main raw material plumbous oxide of PZT base ceramic material is a kind of volatile toxic substance, bring serious harm all can in its production and application and waste treatment process the mankind and ecotope, therefore eco-friendly novel piezo-electric ceramic material has become the focus of world's extensive concern and research and development.Bismuth-sodium titanate base lead-free piezoelectric ceramic is because it has superior piezoelectric property and higher Curie temperature, because of but one of leadless piezoelectric ceramics system at present of greatest concern.
In recent years, the preparation method of bismuth-sodium titanate base lead-free piezoelectric ceramic mainly comprises: conventional solid-state method, hydrothermal synthesis method, sol-gel synthesis method (sol-gel), template grain growth (Templated Grain Growth, TGG), reaction template grain growing method (Reactive-Templated Grain Growth, etc., and different preparation technologies has great impact to ceramic performance RTGG).Wherein, solid sintering technology is one of the most frequently used method, have the features such as preparation technology is simple, cost is low, but the cycle is long, and the ceramic stability of preparing is poor; Sol-gel method preparation cost is low, and the powder particle obtaining is tiny, but technique more complicated; And these two kinds of methods of TGG and RTGG, owing to adopting texturing growing technology, its ceramic anisotropic degree preparing is high, thereby the textured piezoelectric ceramic excellent property obtaining.
At present, the textured piezoelectric ceramic of preparing by casting method is all to adopt non-aqueous tape-casting moulding, because organic content in non-aqueous tape-casting moulding process is more, can cause that ceramic diaphragm density is low, the yielding problems of crack of base substrate in binder removal process, thereby affect quality product, production cost is higher in addition, and use is inflammable, poisonous organic solvent, can cause serious harm to human body and environment, the development trend such as close friend and cleaner production can not conform.For this reason, studying, environmental protection low taking the cost aqueous tape casting forming technique as feature, be not only and adapt to produce and the needs of Economic development, is also an urgent demand of raising social benefit.At present, there is not yet about adopting aqueous tape casting forming technique to prepare the report of bismuth sodium titanate based textured piezoelectric ceramic.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry is provided, be beneficial to realize the preparation of this system material textured piezoelectric ceramic diaphragm, obtain the product of quality and excellent property.Another object of the present invention is to provide a kind of utilizes above-mentioned slurry to adopt aqueous tape casting forming technique to prepare the method for textured piezoelectric ceramic diaphragm.
Object of the present invention is achieved by the following technical programs:
The bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry of one provided by the invention, it consists of: ceramic base-material 32～69wt%, template 1～20wt%, deionized water 15～55wt%, dispersion agent 0.5～5wt%, binding agent 5～35wt%, softening agent 1～10wt%, film coalescence aid 0.01～3wt%, defrother 0.02～1wt%; Described ceramic base-material is the bismuth sodium titanate based ceramic powder containing 1～5wt% sintering aid; Described template is sheet Na
0.5bi
4.5ti
4o
15.Preferably, described slurry its consist of: ceramic base-material 33～60wt%, template 3～15wt%, deionized water 20～50wt%, binding agent 8～25wt%, softening agent 3～8wt%, dispersion agent 1～4wt%, film coalescence aid 0.5～2.5wt%, defrother 0.02～0.1wt%.
Further, sintering aid of the present invention is Bi
2o
3+ CuO+B
2o
3+ ZnO+MnO
2compound frit, in mass ratio [Bi
2o
3: B
2o
3: CuO]: [ZnO: MnO
2]=3～9: 5～8, wherein Bi
2o
3: B
2o
3: CuO=5～9: 2: 1, ZnO: MnO
2=1: 2～6.Described bismuth sodium titanate based ceramic powder is for having perovskite structure (ABO
3) bismuth-sodium titanate, simultaneously composite mixed bismuth potassium titanate, barium titanate and the potassium-sodium niobate lithium with perovskite structure, its general structure is:
(1-x-y-z) Na
0.5bi
0.5tiO
3-yK
0.5bi
0.5tiO
3-xBaTiO
3-zK
ana
bli
1-a-bnbO
3, wherein 0≤x≤0.2,0.01≤y≤0.5,0≤z≤0.5,0≤a≤0.5,0≤b≤0.5.
Further, the particle diameter of ceramic base-material of the present invention is 0.01～4 μ m.Described sheet Na
0.5bi
4.5ti
4o
15its sheet-like morphology is thick 0.5～3 μ m, radially long 10～45 μ m.
In such scheme, dispersion agent of the present invention is polyoxyethylene glycol, and described binding agent is polyvinyl alcohol, and described softening agent is glycerine, and described film coalescence aid is tributyl phosphate, and described defrother is alkyl-silicone oil or propyl carbinol.
Another object of the present invention is achieved by the following technical programs:
The preparation method of a kind of bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting ceramic diaphragm provided by the invention, adopts above-mentioned bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry, comprises the following steps:
(1) deionized water that contains dispersion agent is joined in ceramic base-material and stirs 5～16h, add afterwards template to stir 2～5h; Then add binding agent, softening agent to stir 3～6h; Finally add film coalescence aid and defrother to stir 0.5～2h, obtain aqueous casting slurry;
(2) will after described aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.1～1m/min, and casting films thickness is 50～300 μ m;
(3) by the diaphragm of described flow casting molding dry 1～24h at 30～80 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
The present invention has following beneficial effect:
The present invention adopts the solvent of deionized water as casting slurry, replace inflammable and explosive, poisonous organic solvent, the development trend such as close friend and cleaner production well not only can conform, and avoided that the diaphragm density that causes because organic content is more in non-aqueous tape-casting moulding process is low, the yielding cracking of base substrate affects the problems such as quality product in binder removal process, the curtain coating ceramic diaphragm obtaining has that even structure, smooth surface, intensity are high, good toughness, be convenient to the premium propertiess such as cutting and processing.In addition, water-based flow casting technique cost of the present invention low, use safely, be suitable for large-scale industrial production.
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment
The bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry of the embodiment of the present invention, is made up of ceramic base-material, template, deionized water, organic additive.
Pottery base-material is for containing 1～5wt% sintering aid (Bi
2o
3+ CuO+B
2o
3+ ZnO+MnO
2compound frit) bismuth sodium titanate based ceramic powder, its particle diameter is 0.01～4 μ m; Wherein bismuth sodium titanate based ceramic powder is for having perovskite structure (ABO
3) bismuth-sodium titanate, simultaneously composite mixed bismuth potassium titanate, barium titanate and the potassium-sodium niobate lithium with perovskite structure, its general structure is:
(1-x-y-z) Na
0.5bi
0.5tiO
3-yK
0.5bi
0.5tiO
3-xBaTiO
3-zK
ana
bli
1-a-bnbO
3, wherein 0≤x≤0.2,0.01≤y≤0.5,0≤z≤0.5,0≤a≤0.5,0≤b≤0.5.
Template is that having thick is 0.5～3 μ m, the Na that radially grows 10～45 μ m sheet-like morphologies
0.5bi
4.5ti
4o
15.
Organic additive is as follows: dispersion agent is polyoxyethylene glycol, and binding agent is polyvinyl alcohol, and softening agent is glycerine, and film coalescence aid is tributyl phosphate, and defrother is alkyl-silicone oil or propyl carbinol.
The bismuth sodium titanate based ceramic powder of various embodiments of the present invention, the formulation parameter in its general structure is as shown in table 1.
Formulation parameter in the bismuth sodium titanate based ceramic powder general structure of table 1 embodiment of the present invention
| Embodiment | x | y | z | a | b |
| Embodiment mono- | 0.0050 | 0.01 | 0.10 | 0 | 0.50 |
| Embodiment bis- | 0.0300 | 0.10 | 0.15 | 0.10 | 0.25 |
| Embodiment tri- | 0.0100 | 0.25 | 0.20 | 0.35 | 0.30 |
| Embodiment tetra- | 0.0600 | 0.40 | 0.25 | 0.50 | 0.45 |
| Embodiment five | 0 | 0.35 | 0.30 | 0.25 | 0.05 |
| Embodiment six | 0.1000 | 0.28 | 0 | 0.15 | 0.20 |
| Embodiment seven | 0.1550 | 0.16 | 0.5 | 0.40 | 0.10 |
| Embodiment eight | 0.2000 | 0.22 | 0.4 | 0.20 | 0.15 |
| Embodiment nine | 0.1300 | 0.09 | 0.45 | 0.05 | 0 |
| Embodiment ten | 0.1800 | 0.5 | 0.05 | 0.30 | 0.35 |
Embodiment mono-:
The preparation method of the bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting of the present embodiment ceramic diaphragm is as follows:
(1) 100g is contained to 1.5wt% sintering aid ([Bi in mass ratio
2o
3: B
2o
3: CuO]: [ZnO: MnO
2]=3: 6, wherein Bi
2o
3: B
2o
3: CuO=6: 2: 1, ZnO: MnO
2=1: 3 compound frit) join in the 52g deionized water that contains 2g dispersion agent polyoxyethylene glycol by the bismuth sodium titanate based ceramic powder of table 1 parameter proportioning, under 400r/min rotating speed, be uniformly mixed 10h, then add 5g sheet Na
0.5bi
4.5ti
4o
15template continues to stir 3h under 100r/min rotating speed; Add afterwards 15g binding agent polyvinyl alcohol, 5g softening agent glycerine to stir 5h under 200r/min rotating speed; Finally add 1.3g film coalescence aid ester tributyl phosphate and 0.09g defrother alkyl-silicone oil to be placed on magnetic stirring apparatus and stir 2h, obtain aqueous casting slurry, its viscosity is 69mPas;
(2) will after aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.5m/min, and casting films thickness is 200 μ m;
(3) by the diaphragm of flow casting molding dry 8h at 60 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
The ceramic diaphragm smooth surface that the present embodiment makes and do not ftracture, good toughness.To after diaphragm cutting, lamination, hot pressing, put into sintering oven, rise to 650 DEG C with the speed of 0.5 DEG C/min and carry out binder removal, insulation 2h; Then the plain sheet that sequences glue being risen to 1100 DEG C of insulation 5h with the speed of 3 DEG C/min can sintering, by silver, polarization, test.Record the piezoelectric constant d of textured piezoelectric ceramic
33=179pC/N, electromechanical coupling factor k
p=31.7%.
Embodiment bis-:
The preparation method of the bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting of the present embodiment ceramic diaphragm is as follows:
(1) 100g is contained to 1.0wt% sintering aid ([Bi in mass ratio
2o
3: B
2o
3: CuO]: [ZnO: MnO
2]=3: 8, wherein Bi
2o
3: B
2o
3: CuO=9: 2: 1, ZnO: MnO
2=1: 4 compound frit) join in the 48g deionized water that contains 3g dispersion agent polyoxyethylene glycol by the bismuth sodium titanate based ceramic powder of table 1 parameter proportioning, under 400r/min rotating speed, be uniformly mixed 12h, then add 10g sheet Na
0.5bi
4.5ti
4o
15template continues to stir 4h under 100r/min rotating speed; Add afterwards 20g binding agent polyvinyl alcohol, 6g softening agent glycerine to stir 5h under 200r/min rotating speed; Finally add 2g film coalescence aid ester tributyl phosphate and 0.06g defrother alkyl-silicone oil to be placed on magnetic stirring apparatus and stir 2h, obtain aqueous casting slurry, its viscosity is 75mPas;
(2) will after aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.6m/min, and casting films thickness is 250 μ m;
(3) by the diaphragm of flow casting molding dry 8h at 60 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
The ceramic diaphragm smooth surface that the present embodiment makes and do not ftracture, good toughness.To after diaphragm cutting, lamination, hot pressing, put into sintering oven, rise to 650 DEG C with the speed of 0.5 DEG C/min and carry out binder removal, insulation 2h; Then the plain sheet that sequences glue being risen to 1120 DEG C of insulation 5h with the speed of 3 DEG C/min can sintering, by silver, polarization, test.Record the piezoelectric constant d of textured piezoelectric ceramic
33=187pC/N, electromechanical coupling factor k
p=30.7%.
Embodiment tri-:
The preparation method of the bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting of the present embodiment ceramic diaphragm is as follows:
(1) 100g is contained to 2.0wt% sintering aid ([Bi in mass ratio
2o
3: B
2o
3: CuO]: [ZnO: MnO
2wherein Bi of]=7: 5
2o
3: B
2o
3: CuO=6: 2: 1, ZnO: MnO
2=1: 5 compound frit) join in the 45g deionized water that contains 2g dispersion agent polyoxyethylene glycol by the bismuth sodium titanate based ceramic powder of table 1 parameter proportioning, under 400r/min rotating speed, be uniformly mixed 8h, then add 10g sheet Na
0.5bi
4.5ti
4o
15template continues to stir 3h under 100r/min rotating speed; Add afterwards 22g binding agent polyvinyl alcohol, 7g softening agent glycerine to stir 5h under 200r/min rotating speed; Finally add 1.3g film coalescence aid ester tributyl phosphate and 0.09g defrother propyl carbinol to be placed on magnetic stirring apparatus and stir 1h, obtain aqueous casting slurry, its viscosity is 87mPas;
(2) will after aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.5m/min, and casting films thickness is 170 μ m;
(3) by the diaphragm of flow casting molding dry 12h at 65 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
The ceramic diaphragm smooth surface that the present embodiment makes and do not ftracture, good toughness.To after diaphragm cutting, lamination, hot pressing, put into sintering oven, rise to 650 DEG C with the speed of 0.5 DEG C/min and carry out binder removal, insulation 2h; Then the plain sheet that sequences glue being risen to 1120 DEG C of insulation 5h with the speed of 3 DEG C/min can sintering, by silver, polarization, test.Record the piezoelectric constant d of textured piezoelectric ceramic
33=205pC/N, electromechanical coupling factor k
p=32..9%.
Embodiment tetra-:
The preparation method of the bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting of the present embodiment ceramic diaphragm is as follows:
(1) 100g is contained to 4wt% sintering aid ([Bi in mass ratio
2o
3: B
2o
3: CuO]: [ZnO: MnO
2]=8: 6, wherein Bi
2o
3: B
2o
3: CuO=7: 2: 1, ZnO: MnO
2=1: 2 compound frit) join in the 39g deionized water that contains 2.5g dispersion agent polyoxyethylene glycol by the bismuth sodium titanate based ceramic powder of table 1 parameter proportioning, under 400r/min rotating speed, be uniformly mixed 10h, then add 12g sheet Na
0.5bi
4.5ti
4o
15template continues to stir 3h under 100r/min rotating speed; Add afterwards 19g binding agent polyvinyl alcohol, 4g softening agent glycerine to stir 3h under 200r/min rotating speed; Finally add 2g film coalescence aid ester tributyl phosphate and 0.1g defrother alkyl-silicone oil to be placed on magnetic stirring apparatus and stir 2h, obtain aqueous casting slurry, its viscosity is 79mPas;
(2) will after aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.8m/min, and casting films thickness is 160 μ m;
(3) by the diaphragm of flow casting molding dry 18h at 50 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
The ceramic diaphragm smooth surface that the present embodiment makes and do not ftracture, good toughness.To after diaphragm cutting, lamination, hot pressing, put into sintering oven, rise to 650 DEG C with the speed of 0.5 DEG C/min and carry out binder removal, insulation 2h; Then the plain sheet that sequences glue being risen to 1130 DEG C of insulation 5h with the speed of 3 DEG C/min can sintering, by silver, polarization, test.Record the piezoelectric constant d of textured piezoelectric ceramic
33=187pC/N, electromechanical coupling factor k
p=32.5%.
Embodiment five:
The preparation method of the bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting of the present embodiment ceramic diaphragm is as follows:
(1) 100g is contained to 3wt% sintering aid ([Bi in mass ratio
2o
3: B
2o
3: CuO]: [ZnO: MnO
2]=4: 7, wherein Bi
2o
3: B
2o
3: CuO=6: 2: 1, ZnO: MnO
2=1: 5 compound frit) join in the 29g deionized water that contains 4g dispersion agent polyoxyethylene glycol by the bismuth sodium titanate based ceramic powder of table 1 parameter proportioning, under 400r/min rotating speed, be uniformly mixed 16h, then add 14g sheet Na
0.5bi
4.5ti
4o
15template continues to stir 2h under 100r/min rotating speed; Add afterwards 25g binding agent polyvinyl alcohol, 5g softening agent glycerine to stir 5h under 200r/min rotating speed; Finally add 3g film coalescence aid ester tributyl phosphate and 0.07g defrother alkyl-silicone oil to be placed on magnetic stirring apparatus and stir 0.5h, obtain aqueous casting slurry, its viscosity is 92mPas;
(2) will after aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.5m/min, and casting films thickness is 100 μ m;
(3) by the diaphragm of flow casting molding dry 20h at 40 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
The ceramic diaphragm smooth surface that the present embodiment makes and do not ftracture, good toughness.To after diaphragm cutting, lamination, hot pressing, put into sintering oven, rise to 650 DEG C with the speed of 0.5 DEG C/min and carry out binder removal, insulation 2h; Then the plain sheet that sequences glue being risen to 1100 DEG C of insulation 5h with the speed of 3 DEG C/min can sintering, by silver, polarization, test.Record the piezoelectric constant d of textured piezoelectric ceramic
33=235pC/N, electromechanical coupling factor k
p=34.6%.
Embodiment six:
The preparation method of the bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting of the present embodiment ceramic diaphragm is as follows:
(1) 100g is contained to 2.5wt% sintering aid ([Bi in mass ratio
2o
3: B
2o
3: CuO]: [ZnO: MnO
2]=6: 5, wherein Bi
2o
3: B
2o
3: CuO=8: 2: 1, ZnO: MnO
2=1: 5 compound frit) join in the 35g deionized water that contains 3g dispersion agent polyoxyethylene glycol by the bismuth sodium titanate based ceramic powder of table 1 parameter proportioning, under 400r/min rotating speed, be uniformly mixed 10h, then add 13g sheet Na
0.5bi
4.5ti
4o
15template continues to stir 3h under 100r/min rotating speed; Add afterwards 10g binding agent polyvinyl alcohol, 5g softening agent glycerine to stir 5h under 200r/min rotating speed; Finally add 1.3g film coalescence aid ester tributyl phosphate and 0.09g defrother propyl carbinol to be placed on magnetic stirring apparatus and stir 2h, obtain aqueous casting slurry, its viscosity is 90mPas;
(2) will after aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.3m/min, and casting films thickness is 80 μ m;
(3) by the diaphragm of flow casting molding dry 18h at 50 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
The ceramic diaphragm smooth surface that the present embodiment makes and do not ftracture, good toughness.To after diaphragm cutting, lamination, hot pressing, put into sintering oven, rise to 650 DEG C with the speed of 0.5 DEG C/min and carry out binder removal, insulation 2h; Then the plain sheet that sequences glue being risen to 1130 DEG C of insulation 5h with the speed of 3 DEG C/min can sintering, by silver, polarization, test.Record the piezoelectric constant d of textured piezoelectric ceramic
33=196pC/N, electromechanical coupling factor k
p=35.7%.
Embodiment seven:
The preparation method of the bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting of the present embodiment ceramic diaphragm is as follows:
(1) 100g is contained to 2wt% sintering aid ([Bi in mass ratio
2o
3: B
2o
3: CuO]: [ZnO: MnO
2]=6: 7, wherein Bi
2o
3: B
2o
3: CuO=7: 2: 1, ZnO: MnO
2=1: 6 compound frit) join in the 43g deionized water that contains 1.8g dispersion agent polyoxyethylene glycol by the bismuth sodium titanate based ceramic powder of table 1 parameter proportioning, under 400r/min rotating speed, be uniformly mixed 5h, then add 8g sheet Na
0.5bi
4.5ti
4o
15template continues to stir 5h under 100r/min rotating speed; Add afterwards 15g binding agent polyvinyl alcohol, 5g softening agent glycerine to stir 6h under 200r/min rotating speed; Finally add 1.6g film coalescence aid ester tributyl phosphate and 0.03g defrother alkyl-silicone oil to be placed on magnetic stirring apparatus and stir 2h, obtain aqueous casting slurry, its viscosity is 67mPas;
(2) will after aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.5m/min, and casting films thickness is 280 μ m;
(3) by the diaphragm of flow casting molding dry 8h at 60 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
The ceramic diaphragm smooth surface that the present embodiment makes and do not ftracture, good toughness.To after diaphragm cutting, lamination, hot pressing, put into sintering oven, rise to 650 DEG C with the speed of 0.5 DEG C/min and carry out binder removal, insulation 2h; Then the plain sheet that sequences glue being risen to 1100 DEG C of insulation 5h with the speed of 3 DEG C/min can sintering, by silver, polarization, test.Record the piezoelectric constant d of textured piezoelectric ceramic
33=265pC/N, electromechanical coupling factor k
p=32.6%.
Embodiment eight:
The preparation method of the bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting of the present embodiment ceramic diaphragm is as follows:
(1) 100g is contained to 2wt% sintering aid ([Bi in mass ratio
2o
3: B
2o
3: CuO]: [ZnO: MnO
2]=6: 7, wherein Bi
2o
3: B
2o
3: CuO=6: 2: 1, ZnO: MnO
2=1: 3 compound frit) join in the 32g deionized water that contains 2g dispersion agent polyoxyethylene glycol by the bismuth sodium titanate based ceramic powder of table 1 parameter proportioning, under 400r/min rotating speed, be uniformly mixed 10h, then add 7g sheet Na
0.5bi
4.5ti
4o
15template continues to stir 2h under 100r/min rotating speed; Add afterwards 18g binding agent polyvinyl alcohol, 5g softening agent glycerine to stir 5h under 200r/min rotating speed; Finally add 3g film coalescence aid ester tributyl phosphate and 0.09g defrother propyl carbinol to be placed on magnetic stirring apparatus and stir 2h, obtain aqueous casting slurry, its viscosity is 90mPas;
(2) will after aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.5m/min, and casting films thickness is 230 μ m;
(3) by the diaphragm of flow casting molding dry 5h at 80 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
The ceramic diaphragm smooth surface that the present embodiment makes and do not ftracture, good toughness.To after diaphragm cutting, lamination, hot pressing, put into sintering oven, rise to 650 DEG C with the speed of 0.5 DEG C/min and carry out binder removal, insulation 2h; Then the plain sheet that sequences glue being risen to 1120 DEG C of insulation 5h with the speed of 3 DEG C/min can sintering, by silver, polarization, test.Record the piezoelectric constant d of textured piezoelectric ceramic
33=247pC/N, electromechanical coupling factor k
p=36.3%.
Embodiment nine:
The preparation method of the bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting of the present embodiment ceramic diaphragm is as follows:
(1) 100g is contained to 3wt% sintering aid ([Bi in mass ratio
2o
3: B
2o
3: CuO]: [ZnO: MnO
2]=4: 5, wherein Bi
2o
3: B
2o
3: CuO=7: 2: 1, ZnO: MnO
2=1: 4 compound frit) join in the 35g deionized water that contains 2.5g dispersion agent polyoxyethylene glycol by the bismuth sodium titanate based ceramic powder of table 1 parameter proportioning, under 400r/min rotating speed, be uniformly mixed 10h, then add 10g sheet Na
0.5bi
4.5ti
4o
15template continues to stir 3h under 100r/min rotating speed; Add afterwards 19g binding agent polyvinyl alcohol, 5g softening agent glycerine to stir 5h under 200r/min rotating speed; Finally add 1.5g film coalescence aid ester tributyl phosphate and 0.03g defrother alkyl-silicone oil to be placed on magnetic stirring apparatus and stir 2h, obtain aqueous casting slurry, its viscosity is 86mPas;
(2) will after aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.5m/min, and casting films thickness is 160 μ m;
(3) by the diaphragm of flow casting molding dry 8h at 60 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
The ceramic diaphragm smooth surface that the present embodiment makes and do not ftracture, good toughness.To after diaphragm cutting, lamination, hot pressing, put into sintering oven, rise to 650 DEG C with the speed of 0.5 DEG C/min and carry out binder removal, insulation 2h; Then the plain sheet that sequences glue being risen to 1120 DEG C of insulation 5h with the speed of 3 DEG C/min can sintering, by silver, polarization, test.Record the piezoelectric constant d of textured piezoelectric ceramic
33=189pC/N, electromechanical coupling factor k
p=38.7%.
Embodiment ten:
The preparation method of the bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting of the present embodiment ceramic diaphragm is as follows:
(1) 100g is contained to 3.5wt% sintering aid ([Bi in mass ratio
2o
3: B
2o
3: CuO]: [ZnO: MnO
2]=4: 7, wherein Bi
2o
3: B
2o
3: CuO=6: 2: 1, ZnO: MnO
2=1: 2 compound frit) join in the 39g deionized water that contains 2g dispersion agent polyoxyethylene glycol by the bismuth sodium titanate based ceramic powder of table 1 parameter proportioning, under 400r/min rotating speed, be uniformly mixed 10h, then add 5g sheet Na
0.5bi
4.5ti
4o
15template continues to stir 3h under 100r/min rotating speed; Add afterwards 15g binding agent polyvinyl alcohol, 8g softening agent glycerine to stir 5h under 200r/min rotating speed; Finally add 2g film coalescence aid ester tributyl phosphate and 0.06g defrother propyl carbinol to be placed on magnetic stirring apparatus and stir 2h, obtain aqueous casting slurry, its viscosity is 74mPas;
(2) will after aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.5m/min, and casting films thickness is 90 μ m;
(3) by the diaphragm of flow casting molding dry 8h at 70 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
The ceramic diaphragm smooth surface that the present embodiment makes and do not ftracture, good toughness.To after diaphragm cutting, lamination, hot pressing, put into sintering oven, rise to 650 DEG C with the speed of 0.5 DEG C/min and carry out binder removal, insulation 2h; Then the plain sheet that sequences glue being risen to 1130 DEG C of insulation 5h with the speed of 3 DEG C/min can sintering, by silver, polarization, test.Record the piezoelectric constant d of textured piezoelectric ceramic
33=238pC/N, electromechanical coupling factor k
p=37.6%.
The preparation method of a kind of bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry of the present invention and ceramic diaphragm thereof, its composition consumption and processing parameter are not limited to the above-mentioned embodiment enumerating.
Claims (6)
1. a bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry, it consists of to it is characterized in that described slurry: ceramic base-material 32～69wt%, template 1～20wt%, deionized water 15～55wt%, dispersion agent polyoxyethylene glycol 0.5～5wt%, binding agent polyvinyl alcohol 5～35wt%, softening agent glycerine 1～10wt%, film coalescence aid tributyl phosphate 0.01～3wt%, defrother alkyl-silicone oil or propyl carbinol 0.02～1wt%; Described ceramic base-material is the bismuth sodium titanate based ceramic powder containing 1～5wt% sintering aid, and described bismuth sodium titanate based ceramic powder is (1-x-y-z) Na
0.5bi
0.5tiO
3-yK
0.5bi
0.5tiO
3-xBaTiO
3-zK
ana
bli
1-a-bnbO
3, wherein 0≤x≤0.2,0.01≤y≤0.5,0≤z≤0.5,0≤a≤0.5,0≤b≤0.5; Described template is sheet Na
0.5bi
4.5ti
4o
15.
2. bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry according to claim 1, it consists of to it is characterized in that described slurry: ceramic base-material 33～60wt%, template 3～15wt%, deionized water 20～50wt%, binding agent 8～25wt%, softening agent 3～8wt%, dispersion agent 1～4wt%, film coalescence aid 0.5～2.5wt%, defrother 0.02～0.1wt%.
3. bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry according to claim 1 and 2, is characterized in that: described sintering aid is Bi
2o
3+ CuO+B
2o
3+ ZnO+MnO
2compound frit, in mass ratio [Bi
2o
3: B
2o
3: CuO]: [ZnO: MnO
2]=3～9: 5～8, wherein Bi
2o
3: B
2o
3: CuO=5～9: 2: 1, ZnO: MnO
2=1: 2～6.
4. bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry according to claim 1 and 2, is characterized in that: the particle diameter of described ceramic base-material is 0.01～4 μ m.
5. bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry according to claim 1 and 2, is characterized in that: described sheet Na
0.5bi
4.5ti
4o
15its sheet-like morphology is thick 0.5～3 μ m, radially long 10～45 μ m.
6. a preparation method for bismuth sodium titanate based textured piezoelectric ceramic water-based tape casting ceramic diaphragm, is characterized in that: adopt one of claim 1-5 described bismuth sodium titanate based textured piezoelectric ceramic aqueous casting slurry, comprise the following steps:
(1) deionized water that contains dispersion agent is joined in ceramic base-material and stirs 5～16h, add afterwards template to stir 2～5h; Then add binding agent, softening agent to stir 3～6h; Finally add film coalescence aid and defrother to stir 0.5～2h, obtain aqueous casting slurry;
(2) will after described aqueous casting slurry froth in vacuum, on casting machine, carry out flow casting molding, curtain coating speed is 0.1～1m/min, and casting films thickness is 50～300 μ m;
(3) by the diaphragm of described flow casting molding dry 1～24h at 30～80 DEG C of temperature, then demoulding, obtains ceramic diaphragm.
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| CN101020608A (en) * | 2006-12-11 | 2007-08-22 | 中国科学院上海硅酸盐研究所 | Lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic and its prepn process |
| CN101028979A (en) * | 2006-02-27 | 2007-09-05 | 西北工业大学 | Lead-free piezoelectric knitting ceramic of titanic acid bismuth sodium-titanic acid bismuth potassium and its production |
| CN101217180A (en) * | 2008-01-09 | 2008-07-09 | 华中科技大学 | A preparation method for lead-free piezoelectricity thick film |
| CN102120703A (en) * | 2010-01-11 | 2011-07-13 | 佛山市华南精细陶瓷技术研究开发中心 | High solid content lithium-niobium-titanium series microwave medium ceramic water-based casting green tape |
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| CN101028979A (en) * | 2006-02-27 | 2007-09-05 | 西北工业大学 | Lead-free piezoelectric knitting ceramic of titanic acid bismuth sodium-titanic acid bismuth potassium and its production |
| CN101020608A (en) * | 2006-12-11 | 2007-08-22 | 中国科学院上海硅酸盐研究所 | Lead-less piezoelectric sodium bismuth titanate-bariumtitanate ceramic and its prepn process |
| CN101217180A (en) * | 2008-01-09 | 2008-07-09 | 华中科技大学 | A preparation method for lead-free piezoelectricity thick film |
| CN102120703A (en) * | 2010-01-11 | 2011-07-13 | 佛山市华南精细陶瓷技术研究开发中心 | High solid content lithium-niobium-titanium series microwave medium ceramic water-based casting green tape |
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