CN106565239B - Low-sintering-temperature power type piezoelectric ceramic material and preparation method thereof - Google Patents
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Abstract
The invention relates to a low sintering temperature power type piezoelectric ceramic material and a preparation method thereof, wherein the piezoelectric ceramic material has a chemical general formula as follows: pb1‑xMx(Ni1/2W1/2)y(Mn1/3Sb2/3)z(ZreTif)1‑y‑zO3+awt%Fe2O3+bwt%Sm2O3+cwt%MnO2+ dwt% CuO, wherein: m is Sr2+And/or Ba2+(ii) a x = 0.02-0.1, y = 0-0.1, z = 0.01-0.1, e = 0.40-0.60, f = 0.40-0.60 and satisfies e + f = 1; a =0.01 ~ 0.4, b =0.01 ~ 0.4, c =0.01 ~ 0.4, d =0.1 ~ 0.4. The low sintering temperature piezoelectric ceramic material has the advantages of low sintering temperature, high piezoelectric performance, high mechanical quality factor, high electromechanical coupling coefficient, moderate dielectric constant and low dielectric loss.
Description
Technical Field
The invention relates to the field of piezoelectric ceramics, in particular to a low sintering temperature power type piezoelectric ceramic material and a preparation method thereof.
Background
In recent years, piezoelectric ceramic components have been developed in a direction of miniaturization, integration of the entire device, high performance, multi-functionalization, and integration in order to meet the demand for the development of surface mount technology for integrated circuits. The low-temperature co-fired ceramic technology is adopted in the integrated circuit surface assembly technology, so that on one hand, the assembly density can be improved, the volume is reduced, the weight is reduced, on the other hand, the reliability and the performance can be improved, and the assembly period is further shortened. And laminated ceramics is one of the research hotspots therein. At present, two methods are mainly used for realizing the laminated structure, one method is to sinter a single piece and then bond the laminated structure, and the other method is to laminate and sinter a plurality of layers once, and noble metals such as Pt, Pd and the like are used as inner electrodes. The former reduces the overall performance of the device and the latter is expensive. In order to reduce the cost of the multilayer ceramic device, silver electrode paste having good conductivity and low price is generally used as the internal electrode. Because the melting point of silver is relatively low, the excessive sintering temperature can cause silver ions to diffuse into the ceramic, so that the insulation resistivity of the ceramic is reduced, and the electrical performance of the piezoelectric material is deteriorated. Meanwhile, the low-temperature sintering can effectively inhibit the problems of deviation of stoichiometric ratio, performance reduction and the like caused by volatilization of PbO. In conclusion, the development of low-temperature sintered piezoelectric ceramics is an important research direction for developing laminated piezoelectric ceramics with high reliability, high electrical properties and low cost.
Currently, press forming is the most used forming method in ceramic production. In order to meet the requirements of powder fluidity and filling property for press forming, the formed powder needs to be granulated to form a blank with a certain granularity. The powder formed by spray granulation is an artificial aggregate, which is beneficial to improving the powder fluidity, increasing the molding density and reducing the sintering shrinkage. Spray granulation has many advantages and has become one of the most widely used granulation methods in ceramic production.
Disclosure of Invention
Aiming at the problems and the requirements in the prior art, the invention aims to provide a power type piezoelectric ceramic material with low sintering temperature, high piezoelectric performance, high electromechanical coupling coefficient, moderate dielectric constant and low dielectric loss and a preparation method thereof, and lays a foundation for the application of the piezoelectric ceramic material in a piezoelectric motor.
In one aspect, the present invention provides a low sintering temperature power type piezoelectric ceramic material, which has a chemical general formula: pb1-xMx(Ni1/2W1/2)y(Mn1/3Sb2/3)z(ZreTif)1-y-zO3+awt％Fe2O3+bwt％Sm2O3+cwt％MnO2+ dwt% CuO, wherein: m is Sr2+And/or Ba2+(ii) a x is 0.02 to 0.1, y is 0 to 0.1, z is 0.01 to 0.1, e is 0.40 to 0.60, f is 0.40 to 0.60, and e + f is 1; a is 0.01 to 0.4, b is 0.01 to 0.4, c is 0.01 to 0.4, and d is 0.1 to 0.4.
The low sintering temperature piezoelectric ceramic material has the advantages of low sintering temperature, high piezoelectric performance, high mechanical quality factor, high electromechanical coupling coefficient, moderate dielectric constant and low dielectric loss. The piezoelectric coefficient of the piezoceramic material is d33280 to 326Pc/N, electromechanical coupling coefficient Kp0.55 to 0.60, a dielectric constant εr402 to 820, and a dielectric loss tan delta of 0.48 to 0.86%.
Preferably, M is Sr2+And Ba2+，Sr2+And Ba2+In a molar ratio of 2: 5.
Preferably, the piezoceramic material is in a tetragonal perovskite phase.
On the other hand, the invention also provides a preparation method of the piezoelectric ceramic, which comprises the following steps: synthesizing raw material powder at 700-850 ℃ in an atmospheric atmosphere, performing spray granulation and compression molding, and sintering in air at 960-1040 ℃.
According to the invention, the sintering temperature is low, and the problems that the insulation resistivity of the ceramic is reduced and the electrical performance of the piezoelectric material is deteriorated due to the diffusion of silver ions into the ceramic can be avoided. Meanwhile, the low-temperature sintering can effectively inhibit the problems of deviation of stoichiometric ratio, performance reduction and the like caused by volatilization of PbO.
In addition, the preparation method of the invention adopts a spray granulation mode, thereby improving the powder fluidity, increasing the molding density and reducing the sintering shrinkage. CuO is added as a sintering aid after spray granulation, so that the function of the sintering aid can be better played.
The preparation method has the advantages of simple process, no need of special equipment, low cost and the like, is suitable for large-scale production, and meets the requirement of industrial production.
Preferably, the method comprises the steps of:
a) weighing Pb in stoichiometric ratio3O4、ZrO2、TiO2、MCO3、MnO2、Sm2O3、Sb2O3、Fe2O3、NiO、WO3Raw material powder is ball milled to be evenly mixed, and the MCO3Is SrCO3And/or BaCO3；
b) Drying the mixed powder, pressing into blocks, and synthesizing at 700-850 ℃ in an atmospheric atmosphere;
c) ball-milling and uniformly mixing the synthesized powder, drying, adding a binder, and performing spray granulation to obtain ceramic powder with strong fluidity;
d) pressing the ceramic powder after spray granulation into blocks, removing plastics, crushing, sieving, adding the weighed CuO powder, and performing ball milling to uniformly mix;
e) drying the mixed powder, adding a binder, granulating, aging, sieving, molding and removing plastic to obtain a ceramic blank;
f) sintering the ceramic blank in air: heating to 960-1040 ℃ at the speed of 1-4 ℃/min, and then preserving heat for 2-3 hours; cooling to room temperature along with the furnace to obtain the power type piezoceramic material.
Preferably, the ball milling in the step a) is wet ball milling, the mass ratio of the ball grinding materials to the ball milling medium and the deionized water is 1:1.0: 0.6-1: 1.5:1.2, the ball milling time is 12-24 hours, and the ball milling medium is agate balls.
Preferably, in step b), the synthesis time is 2 to 12 hours.
Preferably, the ball milling in the step c) is wet ball milling, the mass ratio of the ball grinding materials to the ball milling medium and the deionized water is 1:1.0: 0.6-1: 1.5:1.2, the ball milling time is 36-48 hours, and the ball milling medium is agate balls.
Preferably, in the step c) and/or the step e), the binder is a polyvinyl alcohol aqueous solution with the mass fraction of 6-7%, and the addition amount of the polyvinyl alcohol aqueous solution is 5-7% of the mass of the powder.
Drawings
FIGS. 1(a) to 1(d) are SEM photographs of the surfaces of the ceramic materials prepared in examples 1 to 4;
FIG. 2 is an X-ray diffraction chart of the ceramic materials obtained in examples 1 to 4.
Detailed Description
The present invention will be further described with reference to the following embodiments with reference to the accompanying drawings. It is to be understood that these drawings and embodiments are illustrative of the invention and are not to be construed as limiting the invention.
The invention provides a low sintering temperature power type piezoceramic material. The power type piezoceramic material has the following composition general formula: pb1-xMx(Ni1/2W1/2)y(Mn1/3Sb2/3)z(ZreTif)1-y-zO3+awt％Fe2O3+bwt％Sm2O3+cwt％MnO2+ dwt% CuO, wherein: m is Sr2+And/or Ba2+(ii) a x is 0.02 to 0.1, y is 0 to 0.1, z is 0.01 to 0.1, e is 0.40 to 0.60, f is 0.40 to 0.60, and e + f is 1, a is 0.01 to 0.4, b is 0.01 to 0.4, c is 0.01 to 0.4, and d is 0.1 to 0.4. Preferably 0 < y.ltoreq.0.1, more preferably 0.01. ltoreq. y.ltoreq.0.03.
As a preferable mode, M is Sr2+And Ba2+Then, Sr2+And Ba2+In a molar ratio of 2: 5.
The piezoelectric ceramic material has the advantages of low sintering temperature, high piezoelectric performance, high mechanical quality factor, high electromechanical coupling coefficient, moderate dielectric constant and low dielectric loss. The sintering temperature can be 960-1040 ℃, and is preferably 960-1000 ℃. In one example, the piezoelectric coefficient is d33280 to 326Pc/N, electromechanical coupling coefficient Kp0.55 to 0.60, a dielectric constant εr402 to 820, and a dielectric loss tan delta of 0.48 to 0.86%.
The grain size of the piezoceramic material is uniform and small, for example, between 2 and 6 mu m. Moreover, the piezoelectric ceramic material of the present invention is excellent in compactness. The density of the powder can be 7.25 to 7.57g/cm3. In addition, the piezoelectric ceramic material of the present invention is in a tetragonal perovskite phase.
The power type piezoceramic material provided by the invention can be prepared by adopting the traditional solid phase method powder preparation and air sintering process and combining the spray granulation mode. In one example, the raw material powder is synthesized at 700-850 ℃ in an atmospheric atmosphere, then is subjected to spray granulation and molding, and is sintered at 960-1040 ℃ in air.
More specifically, as an example, the following steps may be included:
a) weighing Pb in stoichiometric ratio3O4、ZrO2、TiO2、SrCO3、BaCO3、MnCO3、Sm2O3、Sb2O3、Fe2O3、NiO、WO3Ball milling the raw material powder to uniformly mix;
b) drying the mixed powder, pressing into blocks, and synthesizing at 700-850 ℃ in an atmospheric atmosphere;
c) uniformly mixing the synthesized powder by a wet ball milling method, drying the powder, adding a binder, and performing spray granulation to obtain ceramic powder with strong fluidity;
d) pressing the ceramic powder after spray granulation into blocks, removing plastics, crushing, sieving, adding the weighed CuO powder, and performing ball milling to uniformly mix;
e) drying the mixed powder, adding a binder, granulating, aging, sieving, molding and removing plastic to obtain a ceramic blank;
f) sintering the ceramic blank in air: heating to 960-1040 ℃ at the speed of 1-4 ℃/min, and then preserving heat for 2-3 hours; cooling to room temperature along with the furnace to obtain the power type piezoceramic material.
In step a), the raw material is not limited to the oxide powder or the carbonate powder, and any material that can be converted into an oxide by calcination may be used.
The ball milling in the step a) can be wet ball milling, the mass ratio of ball grinding materials to ball milling media and deionized water is 1:1.0: 0.6-1: 1.5:1.2, the ball milling time is 6 hours, and the ball milling media are agate balls.
In the step b), the synthesis time can be 2-12 hours. In a preferred example, the synthesis time is 6 to 12 hours.
The ball milling in the step c) can be wet ball milling, the mass ratio of ball grinding materials to ball milling media and deionized water is 1:1.0: 0.6-1: 1.5:1.2, the ball milling time is 24 hours, and the ball milling media are agate balls.
In the step c), the binder may be polyvinyl alcohol, for example, a polyvinyl alcohol aqueous solution with a mass fraction of 6-7%, and the addition amount of the polyvinyl alcohol aqueous solution may be 5-7% of the mass of the powder.
In the step c), the grain diameter of the ceramic powder formed by spray granulation can be 40 um-100 um.
In step d), the sieving may be a 40 mesh sieve.
The timing of adding the CuO powder described in step d) is after spray granulation. This can bring the sintering aid into better play.
In the step e), the binder may be polyvinyl alcohol, for example, a polyvinyl alcohol aqueous solution with a mass fraction of 6-7%, and the addition amount of the polyvinyl alcohol aqueous solution may be 5-7% of the mass of the powder. The molding pressure can be 2MPa to 4 MPa.
Compared with the prior art, the invention has the following beneficial effects:
1. the prepared piezoelectric ceramic material with low sintering temperature has the advantages of low sintering temperature, high piezoelectric performance, high mechanical quality factor, high electromechanical coupling coefficient, moderate dielectric constant and small dielectric loss;
2. the preparation method of the invention adopts a spray granulation mode, improves the powder fluidity, increases the molding density and reduces the sintering shrinkage. CuO is added as a sintering aid after spray granulation, so that the function of the sintering aid can be better played;
3. the preparation method has the advantages of simple process, no need of special equipment, low cost and the like, is suitable for large-scale production, and meets the requirement of industrial production.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific parameters of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the parameters within the suitable ranges through the description herein, and are not limited to the specific values of the following examples.
Example 1
Pb0.93Sr0.02Ba0.05(Ni1/2W1/2)0.01(Mn1/3Sb2/3)0.02(Zr0.527Ti0.473)0.97O3+0.01wt％Fe2O3+0.07wt％Sm2O3+0.1wt％MnO2+ 0.1% by weight of CuO piezoceramic material
Weighing Pb in stoichiometric ratio3O4、ZrO2、TiO2、SrCO3、BaCO3、MnCO3、Sm2O3、Sb2O3、Fe2O3、NiO、WO3Raw material powder, and all the powder is uniformly mixed by a wet ball milling process; the ball milling conditions are as follows: and mixing the ball grinding material, the agate balls and the deionized water according to the mass ratio of 1:1.2:1.0, and carrying out ball milling for 24 hours. The obtained mixed powder is pressed into blocks and synthesized in the atmosphere, the synthesis temperature is 850 ℃ and the synthesis time is 2 hours, and the synthesized powder is uniformly mixed by a wet ball milling process after being crushed; the ball milling conditions are as follows: and mixing the ball grinding material, the agate balls and the deionized water according to the mass ratio of 1:1.2:1.0, and carrying out ball milling for 48 hours. Drying the finely ground powder, adding a polyvinyl alcohol (PVA) aqueous solution with the mass fraction of 5 percent and the mass percent of 7 percent of the powder as a binder, spraying, granulating, forming, removing plastic at 800 ℃, crushing, sieving with a 40-mesh sieve, addingAdding CuO powder with the mass ratio of 0.1 wt% into the powder, ball-milling and mixing by a wet method, granulating, molding, removing plastic, heating to 1000 ℃ at the speed of 2 ℃/min, and preserving heat for 2 hours for sintering.
Example 2
Pb0.93Sr0.02Ba0.05(Ni1/2W1/2)0.01(Mn1/3Sb2/3)0.02(Zr0.527Ti0.473)0.97O3+0.01wt％Fe2O3+0.07wt％Sm2O3+0.1wt％MnO2+ 0.2% by weight of CuO piezoceramic material
This embodiment differs from embodiment 1 only in that: adding 0.2 wt% of CuO powder;
the rest of the present example is the same as that described in example 1.
Example 3
Pb0.93Sr0.02Ba0.05(Ni1/2W1/2)0.01(Mn1/3Sb2/3)0.02(Zr0.527Ti0.473)0.97O3+0.01wt％Fe2O3+0.07wt％Sm2O3+0.1wt％MnO2+0.3 wt% CuO piezoceramic material
This embodiment differs from embodiment 1 only in that: adding 0.3 wt% of CuO powder;
the rest of the present example is the same as that described in example 1.
Example 4
Pb0.93Sr0.02Ba0.05(Ni1/2W1/2)0.01(Mn1/3Sb2/3)0.02(Zr0.527Ti0.473)0.97O3+0.01wt％Fe2O3+0.07wt％Sm2O3+0.1wt％MnO2+0.4 wt% CuO piezoceramic material
This embodiment differs from embodiment 1 only in that: adding 0.4 wt% of CuO powder;
the rest of the present example is the same as that described in example 1.
FIGS. 1(a) to (d) are scanning electron micrographs of the surfaces of piezoelectric ceramics obtained in examples 1 to 4. As shown in FIGS. 1(a) to (d), most of the crystal grains of the ceramic have a small size of 2 to 6 μm; the surface of the ceramic sample had pores, but the pores were small and the number was not large, indicating that the ceramic sample had good denseness.
FIG. 2 is an X-ray diffraction chart of the piezoelectric ceramic materials obtained in examples 1 to 4. As can be seen from fig. 2, the piezoelectric ceramic materials obtained in the above examples all have a completely tetragonal perovskite phase.
Table 1 shows the performance data of the piezoceramic materials prepared in examples 1 to 4 and having a sintering temperature of 1000 ℃, wherein the testing method for each parameter is as follows:
density: archimedes method
Piezoelectric coefficient: quasi-static d33Measuring instrument
Electromechanical coupling coefficient: HP4294A impedance analyzer
Dielectric constant and dielectric loss: agilent 4980A.
TABLE 1
As can be seen from table 1: the piezoelectric ceramic material prepared by the method has the advantages of low sintering temperature, high piezoelectric performance, high electromechanical coupling coefficient, moderate dielectric constant and low dielectric loss.
In summary, it can be seen that: the power type piezoelectric ceramic material provided by the invention has the characteristics of low sintering temperature, and also has the advantages of high piezoelectric performance, high electromechanical coupling coefficient, low dielectric loss and the like; the preparation method is simple, does not need special equipment, has low cost, is suitable for large-scale production, and can meet the industrial requirement.
Claims (7)
1. A low sintering temperature power type piezoceramic material is characterized in that the chemical general formula is as follows: pb0.93Sr0.02Ba0.05(Ni1/2W1/2)0.01(Mn1/3Sb2/3)0.02(Zr0.527Ti0.473)0.97O3+0.01wt%Fe2O3+0.07wt%Sm2O3+0.1wt%MnO2, + + dwt% CuO, wherein: d = 0.1-0.4;
the sintering temperature of the piezoceramic material is 960-1040 ℃, and the piezoelectric coefficient of the piezoceramic material is d33280 to 326Pc/N, electromechanical coupling coefficient Kp0.55 to 0.60, a dielectric constant εr402 to 820, a dielectric loss tanδ0.48 to 0.86 percent.
2. The piezoceramic material according to claim 1, wherein the piezoceramic material is in the tetragonal perovskite phase.
3. A method for preparing the low sintering temperature power type piezoceramic material according to claim 1 or 2, comprising the following steps:
a) weighing Pb in stoichiometric ratio3O4、ZrO2、TiO2、SrCO3、BaCO3、MnO2、Sm2O3、Sb2O3、Fe2O3、NiO、WO3Ball milling the raw material powder to uniformly mix;
b) drying the mixed powder, pressing into blocks, and synthesizing at 700-850 ℃ in an atmospheric atmosphere;
c) ball-milling and uniformly mixing the synthesized powder, drying, adding a binder, and performing spray granulation to obtain ceramic powder with strong fluidity;
d) pressing the ceramic powder after spray granulation into blocks, removing plastics, crushing, sieving, adding the weighed CuO powder, and performing ball milling to uniformly mix;
e) drying the mixed powder, adding a binder, granulating, aging, sieving, molding and removing plastic to obtain a ceramic blank;
f) sintering the ceramic blank in air: heating to 960-1040 ℃ at the speed of 1-4 ℃/min, and then preserving heat for 2-3 hours; cooling to room temperature along with the furnace to obtain the power type piezoceramic material.
4. The method according to claim 3, wherein the ball milling in the step a) is wet ball milling, the mass ratio of the ball grinding materials to the ball milling media and the deionized water is 1:1.0: 0.6-1: 1.5:1.2, the ball milling time is 12-24 hours, and the ball milling media are agate balls.
5. The method according to claim 3 or 4, wherein in step b), the synthesis time is 2 to 12 hours.
6. The method according to claim 3 or 4, wherein the ball milling in the step c) is wet ball milling, the mass ratio of ball grinding materials to ball milling media and deionized water is 1:1.0: 0.6-1: 1.5:1.2, the ball milling time is 36-48 hours, and the ball milling media are agate balls.
7. The method according to claim 3 or 4, wherein in the step c) and/or the step e), the binder is a polyvinyl alcohol aqueous solution with the mass fraction of 6-7%, and the addition amount of the polyvinyl alcohol aqueous solution is 5-7% of the mass of the powder.
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| CN101857434A (en) * | 2010-06-04 | 2010-10-13 | 天津大学 | Low-temperature sintered high-power piezoelectric ceramic |
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| CN101857434A (en) * | 2010-06-04 | 2010-10-13 | 天津大学 | Low-temperature sintered high-power piezoelectric ceramic |
| CN103771854A (en) * | 2013-12-20 | 2014-05-07 | 中国科学院上海硅酸盐研究所 | Piezoceramic material and preparation method thereof |
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