CN111925208A - Lithium-sodium niobate-based leadless piezoelectric ceramic and preparation method thereof - Google Patents

Lithium-sodium niobate-based leadless piezoelectric ceramic and preparation method thereof Download PDF

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CN111925208A
CN111925208A CN202010782448.9A CN202010782448A CN111925208A CN 111925208 A CN111925208 A CN 111925208A CN 202010782448 A CN202010782448 A CN 202010782448A CN 111925208 A CN111925208 A CN 111925208A
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ceramic
lithium
ball milling
piezoelectric ceramic
sodium
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王轲
李陈博文
李敬锋
龚文
吴超峰
俞胜平
高洪伟
张丹阳
李庚�
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ZHEJIANG TSINGHUA YANGTZE RIVER DELTA RESEARCH INSTITUTE
Tsinghua University
Goertek Inc
Yangtze Delta Region Institute of Tsinghua University Zhejiang
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ZHEJIANG TSINGHUA YANGTZE RIVER DELTA RESEARCH INSTITUTE
Tsinghua University
Goertek Inc
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Abstract

The invention discloses a sodium lithium niobate-based lead-free piezoelectric ceramic and a preparation method thereof, wherein the sodium lithium niobate-based lead-free piezoelectric ceramic is composed of (1-x) Li shown in the following chemical general formulaαNa1‑αNbO3‑xBaTiO3(ii) a In the preparation process, Li is added2CO3、Na2CO3、Nb2O5、TiO2、BaCO3Mixing, adding absolute ethyl alcohol, ball milling, drying to obtain mixed powder, and presintering the powder; performing secondary ball milling on the pre-sintered powder, and performing cold press molding to obtain a ceramic rough blank; and sintering the ceramic rough blank at a high temperature in an air atmosphere to obtain a ceramic sample, and finally carrying out polarization treatment on the sample to obtain the lithium-sodium niobate-based lead-free piezoelectric ceramic. The lithium niobate sodium-based leadless piezoelectric ceramic prepared by the inventionThe material has the characteristics of high piezoelectric coefficient, high dielectric constant and high electromechanical coupling coefficient, and has the advantages of easily obtained raw materials, simple components, no highly toxic element lead and reduced environmental burden; and the preparation process is simple and consumes short time. The invention has wide application prospect.

Description

Lithium-sodium niobate-based leadless piezoelectric ceramic and preparation method thereof
Technical Field
The invention relates to the field of functional ceramic materials, in particular to a lithium-sodium niobate-based lead-free piezoelectric ceramic and a preparation method thereof.
Background
The piezoelectric material has the capability of converting mechanical energy and electric energy, and is widely applied to the fields of industrial automation, medical care, energy collection and the like, and the application comprises a piezoelectric sensor, an ultrasonic transducer, a piezoelectric driver and the like. Currently, lead zirconate titanate (PZT) -based piezoelectric ceramics have excellent piezoelectric properties and excellent stability, have been widely used in electronic devices, and have been dominant in the market for decades. However, the toxicity of lead in PZT-based materials negatively affects human health and ecosystem, and relevant laws and regulations are issued in countries around the world, such as china, european union, japan, etc., to limit the application of lead in electronic industrial products. Therefore, the research on the high-performance lead-free piezoelectric ceramic material which is environment-friendly and has excellent performance is a subject with great social and economic values.
In 2004, Kimura et al reported that the mechanical quality factor Qm of lithium niobate sodium-based lead-free piezoelectric ceramic treated by annealing is up to 3000, which is comparable to PZT-based piezoelectric ceramic. The discovery of the characteristics also makes the lithium-sodium niobate-based lead-free piezoelectric ceramic receive certain attention and have considerable competitiveness in the application of high-power piezoelectric devices. However, the piezoelectric coefficient d33 is also important for piezoelectric materials, but the lithium sodium niobate-based lead-free piezoelectric ceramics have a large difference from PZT-based lead-free piezoelectric ceramics in this respect. This also seriously affects the progress of practical application of the lithium sodium niobate-based lead-free piezoelectric ceramics.
Disclosure of Invention
The invention aims to provide the lithium-sodium niobate-based lead-free piezoelectric ceramic and the preparation method thereof aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a lithium-sodium niobate based leadless piezoelectric ceramic comprises the chemical composition shown by the following general formula:
(1-x)LiαNa1-αNbO3-xBaTiO3wherein alpha represents the atomic percentage of lithium element in the lithium niobate sodium component and is more than or equal to 0.04 and less than or equal to 0.20, and x represents BaTiO3The x accounts for the atomic percent of the lithium niobate sodium-based lead-free piezoelectric ceramic and is more than or equal to 0 and less than or equal to 0.30.
According to another aspect of the present invention, a method for preparing a lithium sodium niobate based lead-free piezoelectric ceramic is provided, which comprises the following steps:
s1: raw materials are Li according to a chemical formula (1-x)αNa1-αNbO3-xBaTiO3Weighing and mixing the components, adding absolute ethyl alcohol as a medium, and performing ball milling for 8-24 hours to obtain mixed powder;
s2: pre-sintering the mixed powder for 4 hours at the temperature of 900-1100 ℃ in an air atmosphere;
s3: adding absolute ethyl alcohol into the pre-sintered powder as a medium, and carrying out secondary ball milling for 8-24 hours;
s4: performing cold press molding on the powder subjected to secondary ball milling to obtain a ceramic rough blank;
s5: sintering the ceramic rough blank for 1-6 h at 1150-1300 ℃ in air atmosphere to obtain a ceramic sample;
s6: and carrying out polarization treatment on the ceramic sample to obtain the lithium-sodium niobate-based lead-free piezoelectric ceramic.
Preferably, in step S1, the raw material is analytically pure Li2CO3、Na2CO3、Nb2O5、TiO2、BaCO3(ii) a The mass ratio of the absolute ethyl alcohol to the raw materials is 2: 1.
preferably, in step S4, the powder after the secondary ball milling is cold-pressed and molded into a wafer with a diameter of 10mm and a thickness of 1.2-1.5 mm under 50-200 MPa.
Preferably, in step S6, silver electrodes are uniformly coated on both ends of the ceramic sample, the ceramic sample is placed in silicone oil at 60-120 ℃, and then polarization is performed for 15-60 min under the direct-current electric field strength of 3-6 kV/mm.
Preferably, the ball milling is carried out in a ball milling tank, and zirconium dioxide is used for milling balls; sintering is carried out in a covered crucible.
The invention has the beneficial effects that:
1. the invention provides a lithium-sodium niobate based leadless piezoelectric ceramic, which is a novel piezoelectric ceramic with a perovskite structure; aiming at the preparation method provided by the ceramic, the components and the synthesis process are regulated and controlled, and the ceramic has the characteristics of high piezoelectric coefficient, high dielectric constant and high electromechanical coupling coefficient under the process conditions and process parameters, so that the performance of the ceramic can be flexibly regulated and controlled. The results of the specific examples show that the lithium-sodium niobate-based lead-free piezoelectric ceramic prepared by the invention has a forward piezoelectric constant d of 42-110 pC/N at room temperature (25℃)33The electromechanical coupling coefficient can reach 0.47 at most, and the dielectric constant can reach 5000. Obviously, the lithium-sodium niobate-based leadless piezoelectric ceramic has excellent performanceGood piezoelectric performance and comprehensive performance.
2. The lithium sodium niobate leadless piezoelectric ceramic synthesized by the preparation method of the invention does not need the steps of granulation, glue discharge and the like in the traditional piezoelectric ceramic process, thereby shortening the time for synthesizing the ceramic material; the prepared sodium lithium niobate-based lead-free piezoelectric ceramic not only has excellent piezoelectric and dielectric properties, but also has the advantages of easily obtained raw materials, simple components, no highly toxic element lead and reduced environmental burden. Therefore, the lithium niobate sodium-based lead-free piezoelectric ceramic has wide application prospect.
Drawings
Figure 1 is the XRD patterns of example 1 to example 3;
FIG. 2 is a graph showing the change of piezoelectric constant with composition in examples 1 to 3;
FIG. 3 is a graph of the change in dielectric constant with temperature for examples 2, 4 and 5;
FIG. 4 is a simplified process flow diagram of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings and embodiments, and it is to be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are conventionally obtained commercially or prepared by conventional methods.
The invention provides a lithium niobate sodium-based leadless piezoelectric ceramic which has a chemical composition (1-x) Li shown in the following general formulaαNa1-αNbO3-xBaTiO3Wherein x represents BaTiO3X is more than or equal to 0 and less than or equal to 0.30 in the atomic percentage of the lithium-sodium niobate-based lead-free piezoelectric ceramic, and alpha represents the atomic percentage of lithium element in the lithium-sodium niobate component and is more than or equal to 0.04α≤0.20。
The invention also provides a preparation method of the lithium sodium niobate leadless piezoelectric ceramic, which comprises the following steps:
s1: raw materials are Li according to a chemical formula (1-x)αNa1-αNbO3-xBaTiO3Weighing and mixing the components, adding absolute ethyl alcohol as a medium, using zirconium dioxide grinding balls in a ball-milling tank, and carrying out ball milling for 8-24 hours to obtain mixed powder; the starting material used was analytically pure Li2CO3、Na2CO3、Nb2O5、TiO2、BaCO3The mass ratio of the absolute ethyl alcohol to the raw materials is 2: 1;
s2: drying the mixed powder, putting the dried mixed powder into a covered crucible, and presintering the mixture for 4 hours at the temperature of 900-1100 ℃ in an air atmosphere;
s3: adding absolute ethyl alcohol into the pre-sintered powder as a medium, performing secondary ball milling for 8-24 hours, and drying the slurry;
s4: cold-pressing and molding the powder subjected to secondary ball milling into a wafer with the diameter of 10mm and the thickness of 1.2-1.5 mm at 50-200 MPa to obtain a ceramic rough blank;
s5: sintering the ceramic rough blank in a covered crucible for 1-6 h at 1150-1300 ℃ in air atmosphere to obtain a ceramic sample;
s6: and uniformly coating silver electrodes on two ends of the sintered ceramic sample, placing the ceramic sample in silicone oil at the temperature of 60-120 ℃, and polarizing for 15-60 min under the direct-current electric field strength of 3-6 kV/mm.
Example 1:
according to the formula, x is 0 and alpha is 0.12, namely, Li0.12Na0.88NbO3Weighing of analytically pure Li2CO3、Na2CO3、Nb2O5、TiO2、BaCO3。
1) Adding the prepared raw materials into a ball milling tank using absolute ethyl alcohol as a medium, wherein the mass ratio of zirconium dioxide grinding balls to the absolute ethyl alcohol to the raw materials is 2: 1, ball milling for 24 hours, and drying the obtained slurry to obtain mixed powder;
2) putting the mixed powder into a covered crucible, and then presintering the mixed powder in the air for 4 hours at the temperature of 1000 ℃;
3) performing secondary ball milling on the pre-sintered powder for 12 hours and drying the slurry;
4) cold-pressing the powder subjected to the secondary ball milling at 100MPa to form a wafer with the diameter of 10mm and the thickness of 1.4mm to obtain a ceramic rough blank;
5) sintering the ceramic rough blank in a covered crucible for 2 hours at 1210 ℃ in air atmosphere to obtain a ceramic sample;
6) and uniformly coating silver electrodes on two ends of the sintered ceramic sample, placing the ceramic sample in silicone oil at 100 ℃, and polarizing for 30min under the direct-current electric field strength of 5 kV/mm.
Thus, Li is obtained0.12Na0.88NbO3After the lithium-sodium niobate-based lead-free piezoelectric ceramic is placed for 24 hours, a quasi-static piezoelectric coefficient tester is used for testing the piezoelectric performance of the lithium-sodium niobate-based lead-free piezoelectric ceramic, an impedance analyzer is used for testing the electromechanical coupling coefficient of the lithium-sodium niobate-based lead-free piezoelectric ceramic, and the electromechanical coupling coefficient of the lithium-sodium niobate-based lead-free piezoelectric ceramic is 0.47.
FIG. 1 shows the XRD pattern of example 1, from which it can be seen that the sample has a typical orthorhombic perovskite structure;
FIG. 2 shows the piezoelectric constant of example 1, and it can be seen that the piezoelectric constant of the sample at room temperature is 42 pC/N.
Example 2:
with x equal to 0.1 and α equal to 0.12, i.e. formula 0.9Li0.12Na0.88NbO3–0.1BaTiO3Weighing of analytically pure Li2CO3、Na2CO3、Nb2O5、TiO2、BaCO3。
1) Adding the prepared raw materials into a ball milling tank using absolute ethyl alcohol as a medium, wherein the mass ratio of zirconium dioxide grinding balls to the absolute ethyl alcohol to the raw materials is 2: 1, ball milling for 24 hours, and drying the obtained slurry to obtain mixed powder;
2) putting the mixed powder into a covered crucible, and then presintering for 4 hours in the air at the temperature of 1100 ℃;
3) performing secondary ball milling on the pre-sintered powder for 24 hours and drying the slurry;
4) cold-pressing the powder subjected to the secondary ball milling at 200MPa to form a wafer with the diameter of 10mm and the thickness of 1.5mm to obtain a ceramic rough blank;
5) sintering the ceramic rough blank in a covered crucible for 6 hours at 1300 ℃ in air atmosphere to obtain a ceramic sample;
6) and uniformly coating silver electrodes on two ends of the sintered ceramic sample, placing the ceramic sample in silicone oil at 120 ℃, and polarizing for 60min under the direct-current electric field strength of 6 kV/mm.
Thus, 0.9Li was obtained0.12Na0.88NbO3–0.1BaTiO3After the lithium-sodium niobate-based lead-free piezoelectric ceramic is placed for 24 hours, a quasi-static piezoelectric coefficient tester is used for testing the piezoelectric performance of the lithium-sodium niobate-based lead-free piezoelectric ceramic, an impedance analyzer is used for testing the electromechanical coupling coefficient of the lithium-sodium niobate-based lead-free piezoelectric ceramic, and the electromechanical coupling coefficient of a sample is 0.42.
The XRD pattern of example 2 is given in FIG. 1, from which it can be seen that the sample has a typical orthorhombic perovskite structure;
FIG. 2 shows the piezoelectric constant of example 2, from which it can be seen that the piezoelectric constant of the sample at room temperature is 61 pC/N;
the dielectric temperature spectrum of example 2 is given in fig. 3, from which it can be seen that the dielectric constant of the sample at room temperature is 440.
Example 3:
x is 0.124 and α is 0.12, i.e. formula 0.876Li0.12Na0.88NbO3–0.124BaTiO3Weighing of analytically pure Li2CO3、Na2CO3、Nb2O5、TiO2、BaCO3。
1) Adding the prepared raw materials into a ball milling tank using absolute ethyl alcohol as a medium, wherein the mass ratio of zirconium dioxide grinding balls to the absolute ethyl alcohol to the raw materials is 2: 1, ball milling for 20 hours, and drying the obtained slurry to obtain mixed powder;
2) putting the mixed powder into a covered crucible, and then presintering the mixed powder in air at 900 ℃ for 4 hours;
3) performing secondary ball milling on the pre-sintered powder for 20 hours and drying the slurry;
4) cold-pressing the powder subjected to the secondary ball milling at 150MPa to form a wafer with the diameter of 10mm and the thickness of 1.3mm to obtain a ceramic rough blank;
5) sintering the ceramic rough blank in a covered crucible for 3 hours at the temperature of 1200 ℃ in the air atmosphere to obtain a ceramic sample;
6) and uniformly coating silver electrodes on two ends of the sintered ceramic sample, placing the ceramic sample in silicone oil at 120 ℃, and polarizing for 40min under the direct-current electric field strength of 4 kV/mm.
Thus, Li with a chemical formula of 0.876 can be prepared0.12Na0.88NbO3–0.124BaTiO3After the lithium-sodium niobate-based lead-free piezoelectric ceramic is placed for 24 hours, a quasi-static piezoelectric coefficient tester is used for testing the piezoelectric performance of the lithium-sodium niobate-based lead-free piezoelectric ceramic, an impedance analyzer is used for testing the electromechanical coupling coefficient of the lithium-sodium niobate-based lead-free piezoelectric ceramic, and the electromechanical coupling coefficient of the lithium-sodium niobate-based lead-free piezoelectric ceramic is 0.45.
The XRD pattern of example 3 is given in FIG. 1, from which it can be seen that the sample has a typical orthorhombic perovskite structure;
FIG. 2 shows the piezoelectric constant of example 3, and it can be seen that the piezoelectric constant of the sample at room temperature is 110 pC/N.
Example 4:
x is 0.2 and α is 0.12, i.e. formula 0.8Li0.12Na0.88NbO3–0.2BaTiO3Weighing of analytically pure Li2CO3、Na2CO3、Nb2O5、TiO2、BaCO3。
1) Adding the prepared raw materials into a ball milling tank using absolute ethyl alcohol as a medium, wherein the mass ratio of zirconium dioxide grinding balls to the absolute ethyl alcohol to the raw materials is 2: 1, ball milling for 15 hours, and drying the obtained slurry to obtain mixed powder;
2) putting the mixed powder into a covered crucible, and then presintering the mixed powder in air at 1050 ℃ for 4 hours;
3) performing secondary ball milling on the pre-sintered powder for 15 hours and drying the slurry;
4) performing cold pressing molding on the powder subjected to the secondary ball milling at 90MPa to obtain a wafer with the diameter of 10mm and the thickness of 1.2mm to obtain a ceramic rough blank;
5) sintering the ceramic rough blank in a covered crucible for 4 hours at the temperature of 1150 ℃ in the air atmosphere to obtain a ceramic sample;
6) and uniformly coating silver electrodes on two ends of the sintered ceramic sample, placing the ceramic sample in silicone oil at 90 ℃, and polarizing for 30min under the direct-current electric field strength of 5 kV/mm.
Thus, 0.8Li was obtained0.12Na0.88NbO3–0.2BaTiO3After the lithium-sodium niobate-based lead-free piezoelectric ceramic is placed for 24 hours, a quasi-static piezoelectric coefficient tester is used for testing the piezoelectric performance of the lithium-sodium niobate-based lead-free piezoelectric ceramic, an impedance analyzer is used for testing the electromechanical coupling coefficient of the lithium-sodium niobate-based lead-free piezoelectric ceramic, and the electromechanical coupling coefficient of a sample is 0.43.
The dielectric temperature spectrum of example 4 is given in FIG. 3, from which it can be seen that the sample has a dielectric constant of 945 at room temperature.
Example 5:
according to the formula 0.7Li, x is 0.3 and α is 0.120.12Na0.88NbO3–0.3BaTiO3Weighing of analytically pure Li2CO3、Na2CO3、Nb2O5、TiO2、BaCO3。
1) Adding the prepared raw materials into a ball milling tank using absolute ethyl alcohol as a medium, wherein the mass ratio of zirconium dioxide grinding balls to the absolute ethyl alcohol to the raw materials is 2: 1, ball milling for 18 hours, and drying the obtained slurry to obtain mixed powder;
2) putting the mixed powder into a covered crucible, and then presintering the mixed powder in air at 1050 ℃ for 4 hours;
3) performing secondary ball milling on the pre-sintered powder for 18 hours and drying the slurry;
4) cold-pressing the powder subjected to the secondary ball milling at 180MPa to form a wafer with the diameter of 10mm and the thickness of 1.4mm to obtain a ceramic rough blank;
5) sintering the ceramic rough blank in a covered crucible at 1250 ℃ in air atmosphere for 5h to obtain a ceramic sample;
6) and uniformly coating silver electrodes on two ends of the sintered ceramic sample, placing the ceramic sample in silicon oil at the temperature of 110 ℃, and polarizing for 25min under the direct-current electric field strength of 3 kV/mm.
Thus, 0.7Li was obtained0.12Na0.88NbO3–0.3BaTiO3After the lithium-sodium niobate-based lead-free piezoelectric ceramic is placed for 24 hours, a quasi-static piezoelectric coefficient tester is used for testing the piezoelectric performance of the lithium-sodium niobate-based lead-free piezoelectric ceramic, an impedance analyzer is used for testing the electromechanical coupling coefficient of the lithium-sodium niobate-based lead-free piezoelectric ceramic, and the electromechanical coupling coefficient of the lithium-sodium niobate-based lead-free piezoelectric ceramic is 0.45.
The dielectric temperature spectrum of example 5 is shown in FIG. 3, from which it can be seen that the dielectric constant of the sample at room temperature is 3500.
Example 6:
x is 0.4 and α is 0.12, i.e. formula 0.6Li0.12Na0.88NbO3–0.4BaTiO3Weighing of analytically pure Li2CO3、Na2CO3、Nb2O5、TiO2、BaCO3。
1) Adding the prepared raw materials into a ball milling tank using absolute ethyl alcohol as a medium, wherein the mass ratio of zirconium dioxide grinding balls to the absolute ethyl alcohol to the raw materials is 2: 1, ball milling for 22 hours, and drying the obtained slurry to obtain mixed powder;
2) putting the mixed powder into a covered crucible, and then presintering the mixed powder in the air for 4 hours at the temperature of 1000 ℃;
3) performing secondary ball milling on the pre-sintered powder for 22 hours and drying the slurry;
4) cold-pressing and molding the powder subjected to secondary ball milling into a wafer with the diameter of 10mm and the thickness of 1.4mm under 160MPa to obtain a ceramic rough blank;
5) sintering the ceramic rough blank in a covered crucible for 4 hours at 1200 ℃ in air atmosphere to obtain a ceramic sample;
6) and uniformly coating silver electrodes on two ends of the sintered ceramic sample, placing the ceramic sample in silicone oil at 115 ℃, and polarizing for 45min under the direct-current electric field strength of 5 kV/mm.
Thus, 0.6Li was obtained0.12Na0.88NbO3–0.4BaTiO3After the lithium-sodium niobate-based lead-free piezoelectric ceramic is placed for 24 hours, a quasi-static piezoelectric coefficient tester is used for testing the piezoelectric performance of the lithium-sodium niobate-based lead-free piezoelectric ceramic, an impedance analyzer is used for testing the electromechanical coupling coefficient of the lithium-sodium niobate-based lead-free piezoelectric ceramic, and the obtained sample has the electromechanical coupling coefficient of 0.46 and the dielectric constant of 5000.
Compared with the prior art, the method strictly selects the process parameters disclosed by the invention by regulating and controlling the components and the synthesis process, so that the prepared lithium-sodium niobate-based lead-free piezoelectric ceramic has excellent piezoelectric property and comprehensive property and higher application value.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (6)

1. The lithium-sodium niobate-based lead-free piezoelectric ceramic is characterized by comprising the following chemical components in a general formula: (1-x) LiαNa1-αNbO3-xBaTiO3Wherein alpha represents the atomic percentage of lithium element in the lithium niobate sodium component and is more than or equal to 0.04 and less than or equal to 0.20, and x represents BaTiO3The x accounts for the atomic percent of the lithium niobate sodium-based lead-free piezoelectric ceramic and is more than or equal to 0 and less than or equal to 0.30.
2. The method for producing a lithium sodium niobate-based lead-free piezoelectric ceramic according to claim 1, comprising the steps of:
s1: raw materials are Li according to a chemical formula (1-x)αNa1-αNbO3-xBaTiO3Weighing and mixing the components, adding absolute ethyl alcohol as a medium, and performing ball milling for 8-24 hours to obtain mixed powder;
s2: pre-sintering the mixed powder for 4 hours at the temperature of 900-1100 ℃ in an air atmosphere;
s3: adding absolute ethyl alcohol into the pre-sintered powder as a medium, and carrying out secondary ball milling for 8-24 hours;
s4: performing cold press molding on the powder subjected to secondary ball milling to obtain a ceramic rough blank;
s5: sintering the ceramic rough blank for 1-6 h at 1150-1300 ℃ in air atmosphere to obtain a ceramic sample;
s6: and carrying out polarization treatment on the ceramic sample to obtain the lithium-sodium niobate-based lead-free piezoelectric ceramic.
3. The method according to claim 2, wherein the raw material is analytically pure Li in step S12CO3、Na2CO3、Nb2O5、TiO2、BaCO3(ii) a The mass ratio of the absolute ethyl alcohol to the raw materials is 2: 1.
4. the method of claim 2, wherein in step S4, the powder after the secondary ball milling is cold-pressed at 50-200 MPa to form a wafer with a diameter of 10mm and a thickness of 1.2-1.5 mm.
5. The method according to claim 2, wherein in step S6, the ceramic sample is uniformly coated with silver electrodes at both ends, placed in silicone oil at 60-120 ℃, and then polarized for 15-60 min under a direct current field strength of 3-6 kV/mm.
6. The method of claim 2, wherein the ball milling is carried out in a ball milling jar, zirconia balls; sintering is carried out in a covered crucible.
CN202010782448.9A 2020-08-06 2020-08-06 Lithium-sodium niobate-based leadless piezoelectric ceramic and preparation method thereof Pending CN111925208A (en)

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