CN114249592A - Preparation method of hard piezoelectric ceramic material - Google Patents
Preparation method of hard piezoelectric ceramic material Download PDFInfo
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Abstract
The invention belongs to the technical field of piezoelectric ceramic materials, and particularly relates to a preparation method of a hard piezoelectric ceramic material. The invention prepares the piezoelectric ceramic material by the steps of primary mixing, filter pressing, drying and briquetting, presintering synthesis, secondary mixing, spray granulation, molding, plastic discharging, sintering and polarization treatment by silver electrodes and air, and the prepared piezoelectric ceramic material belongs to hard piezoelectric ceramic, and has the characteristics of high dielectric constant of 1900, high electromechanical coupling coefficient of 0.66, high mechanical quality factor Qm of 1300 and low dielectric loss, can obviously improve the use effect of the piezoelectric ceramic material, has good repeatability and stability, is suitable for batch production, and can be used in the fields of ultrasonic cleaning, ultrasonic atomization, electronic component manufacturing and the like in large batch.
Description
Technical Field
The invention belongs to the technical field of piezoelectric ceramic materials, and particularly relates to a preparation method of a hard piezoelectric ceramic material.
Background
When a voltage is applied to the electrodes of the ceramic plate, the ceramic plate generates a deformation effect. The electric effect is generated due to deformation, and is called as a positive piezoelectric effect; the deformation effect is generated due to the applied voltage, and is called inverse piezoelectric effect. The piezoelectric effect reflects the linear coupling relationship between the "pressure" and "electricity" of the ceramic. The piezoelectric effect of a piezoelectric ceramic is determined by its internal structure, i.e., its interior is made of polycrystalline material. The hard piezoelectric ceramic is prepared by doping PZT ceramic with Pb in electric valence ratio2+Low Na content+、K+Plasma or electrovalence ratio T4+Low Fe2+、Co2+、Ni2+、Cr3+And (3) plasma. After doping, the coercive field Ec of the PZT ceramic is increased, the dielectric constant, Kp and tan delta are reduced, Qm is increased, and the term 'hard' refers to that the correction field Ec is increased after the additives are added, so that under the action of an electric field or stress, both pre-polarization and depolarization are more difficult, and the material property is changed into 'hard'. At present, the highest level dielectric constant 1650, the electromechanical coupling coefficient Kp of the hard piezoelectric ceramics on the market is 0.62, the dielectric loss tan delta is less than or equal to 0.6%, the best level of Qm is 1000, and the performance of the hard piezoelectric ceramics cannot be further improved, so that the application of the hard piezoelectric ceramics is greatly limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a hard piezoelectric ceramic material, aiming at solving the technical problems that the highest level dielectric constant 1650, the electromechanical coupling coefficient Kp of the hard piezoelectric ceramic material on the market is 0.62, the dielectric loss tan delta is less than or equal to 0.6 percent, the best level of Qm is 1000, the performance of the hard piezoelectric ceramic material cannot be further improved, and the application of the hard piezoelectric ceramic material is greatly limited.
The invention provides a preparation method of a hard piezoelectric ceramic material, which has the following specific technical scheme:
the preparation method of the hard piezoelectric ceramic material comprises the following steps:
s1, weighing the following raw materials in percentage by weight: 62-68% of lead tetraoxide, 10-13% of zirconium dioxide, 15-17% of titanium dioxide, 1.5-3.5% of bismuth trioxide, 0.5-1.5% of antimony trioxide and 2-4% of rare earth, mixing the raw materials for the first time to obtain a first mixed slurry, and performing filter pressing dehydration, drying and briquetting and presintering synthesis to obtain a material block;
s2, performing secondary material mixing on the blocks subjected to pre-sintering synthesis in the step S1 to obtain second mixed slurry, performing spray granulation on the second mixed slurry to obtain powder, and performing molding treatment on the powder to obtain a blank;
s3, performing plastic removal and sintering treatment on the blank in the step S2 to obtain a ceramic blank sheet;
s4, subjecting the ceramic blank sheet in the step S3 to silver electrode and air polarization treatment to obtain the hard piezoelectric ceramic material.
In some embodiments, in step S1, the first mixing is to mix and grind the raw materials into slurry with a particle size of 1-3 μm by adding deionized water through a stirring mill. Wherein the weight of the deionized water is 50-70% of the weight of the raw materials, the diameter of the zirconium dioxide ball is 1-15 mm, and the weight of the zirconium dioxide ball is 200% of the weight of the raw materials.
In some embodiments, in the drying briquette treatment in step S1, the drying temperature is 170 ℃ and the briquette pressure is 0.8 ton/cm2The temperature of the pre-sintering synthesis is 800-900 ℃, and the time is 3-5 h.
In some embodiments, in step S2, the second mixing process is to add deionized water into the pre-sintered material block to grind the material block into slurry with a particle size of 1 to 3 μm by using a stirring mill, and then grind the obtained slurry into slurry with a particle size of 0.6 to 0.8 μm by using a sand mill to obtain a second mixed slurry. Wherein the weight of the deionized water is 50-70% of the weight of the raw materials, the diameter of the zirconium dioxide ball is 1-15 mm, and the weight of the zirconium dioxide ball is 200% of the weight of the raw materials. In the dry pressing step, the dry pressing pressure is 2.3 tons/cm2。
In certain embodiments, in step S2, the spray granulation process comprises the following steps: 9% of polyvinyl alcohol (PVA) solution and 1% of surfactant are added into the second mixed slurry, and then the mixture is sent into a spray tower for spray granulation treatment. The preparation method of the PVA solution comprises the following steps: heating PVA 8% and deionized water 92% in water bath at 90 deg.C, stirring to dissolve for 12 hr, and sieving with 250 mesh sieve.
Further, the feeding temperature of the spray tower is 230-250 ℃, and the discharging temperature is 80-100 ℃.
In some embodiments, in step S3, the plastic removing process is to heat the blank to 600-800 ℃ and maintain the temperature for 2-3 h.
In some embodiments, in step S3, an alumina crucible is used for sintering, wherein the sintering temperature is 1250 to 1350 ℃ and the sintering time is 3 to 5 hours.
In some embodiments, in step S4, before being processed by the silver electrode, the ceramic green sheet is subjected to size processing and ultrasonic cleaning, and the processing by the silver electrode is that silver is processed on the upper surface and the lower surface of the ceramic green sheet after size processing, the silver firing temperature is 750-850 ℃, and the silver infiltration temperature is 800 ℃/10 min.
In some embodiments, in step S4, the air polarization treatment is to place the ceramic green sheet processed by the silver electrode in air at 200 ℃ for polarization, the polarization voltage is 1000V/mm, and the pressure is maintained for 30 min.
The invention has the following beneficial effects: according to the preparation method of the hard piezoelectric ceramic material, the growth of piezoelectric ceramic grains can be inhibited by controlling the proportion of lead oxide and zirconium oxide and adding antimony trioxide, so that the void ratio among the grains is reduced, the compactness is improved, the dielectric loss is reduced, the prepared piezoelectric ceramic material belongs to hard piezoelectric ceramic, the Qm value is increased, and the electromechanical coupling coefficient is increased. The ceramic has the characteristics of high dielectric constant which can reach 1900, high electromechanical coupling coefficient which can reach 0.66, mechanical quality factor Qm which can reach 1300 and low dielectric loss, can obviously improve the use effect of the piezoelectric ceramic material, has good repeatability and stability, and is suitable for mass production, thereby being used in the fields of ultrasonic cleaning, ultrasonic atomization, electronic component manufacturing and the like in a large scale.
Drawings
FIG. 1 is a flow chart of a method for preparing a hard piezoelectric ceramic material provided by the present invention;
FIG. 2 is a crystal diagram of product B of example 1 of the present invention at a magnification of 5000 times;
FIG. 3 is a crystallization diagram of product B of example 1 of the present invention magnified 10000 times;
FIG. 4 is a crystal diagram of product E of example 1 of the present invention, magnified 5000 times;
FIG. 5 is a crystallization diagram of product E of example 1 of the present invention magnified 10000 times;
FIG. 6 is a crystal diagram of product H of example 1 of the present invention at 5000 Xmagnification;
FIG. 7 is a crystallization diagram of product H of example 1 of the present invention magnified 10000 times.
Detailed Description
In order that the objects, aspects and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the following detailed description of preferred embodiments thereof, with reference to the accompanying drawings of fig. 1-7.
Example 1
The preparation method of the hard piezoelectric ceramic material provided by the embodiment has the following specific technical scheme:
respectively weighing 98kgPb by using an electronic balance3O4Powder, 17kgZrO2Powder, 24kg TiO2Powder, 3.5kgBi2O3Powder, 2kgSb2O3And 5.5kg of rare earth powder prepared by mixing Pb3O4、ZrO2、TiO2、Bi2O3、Sb2O3Pouring the raw material of the rare earth powder into a stirring mill, taking deionized water as a mixed medium and zirconia balls as a ball milling medium, mixing materials for 5 hours by using the stirring mill, controlling the particle size of the powder to be 1-3 mu m, taking out first mixed slurry, pumping the first mixed slurry into a filter press for pressure filtration and dehydration, putting the dehydrated slurry into a drying box, pressing the slurry into blocks at the temperature of 170 ℃ and the briquetting pressure of 0.8 ton/cm2And drying and briquetting. And then, the dried slurry is subjected to open presintering, the presintering temperature is controlled at 800 ℃, and the presintering heat preservation time is 4 hours. Putting the pre-sintered material blocks into a stirring mill for secondary mixing, wherein the ball milling time is 5 hours, then putting the slurry into a sand mill, circulating for 5 times, controlling the particle size of the powder to be 0.6-0.8 mu m, adding 9% of PVA and 1% of surfactant (emulsifying wax) into the obtained second mixed slurry, stirring, placing the mixture into a storage barrel, controlling the temperature of the slurry entering a spray tower to be 230-250 ℃, and discharging the mixture to be 80-100 ℃, and performing spray granulation. Dry pressing the granulated powder, keeping the temperature at 750 ℃ for 3h to remove glue to obtain a formed blank, sealing the formed blank in an alumina crucible, sintering the blank in a program temperature control box furnace at 1290 ℃ for 4h to obtain a ceramic wafer with the outer diameter of 20mm, grinding the ceramic wafer to the thickness of 1.5mm, cleaning, carrying out electrode impregnation on two surfaces at the temperature of 800 ℃/10min, and finally carrying out air polarization on the ceramic wafer(the polarization medium is air, the polarization temperature is 200 ℃, the polarization voltage is 1000V/mm, the pressure is maintained for 30min), the polarization is stabilized for 3 days, and the piezoelectric performance is tested to obtain a product A.
The preparation method is adopted, the difference is that the presintering temperature is 850 ℃, and the product B is obtained.
The preparation method is adopted, the difference is that the presintering temperature is 900 ℃, and the product C is obtained.
The preparation method is adopted, the difference is only that the sintering temperature is 1330 ℃, and the product D is obtained.
The preparation method is adopted, and the differences are that the presintering temperature is 850 ℃, the sintering temperature is 1330 ℃, and the product E is obtained.
The preparation method is adopted, and the differences are that the presintering temperature is 900 ℃, the sintering temperature is 1330 ℃, and the product F is obtained.
The preparation method is adopted, the difference is that the sintering temperature is 1260 ℃, and the product G is obtained.
The preparation method is adopted, and the differences are that the presintering temperature is 850 ℃, the sintering temperature is 1260 ℃, and the product H is obtained.
The preparation method is adopted, and the differences are that the presintering temperature is 900 ℃, the sintering temperature is 1260 ℃, and the product I is obtained.
Example 2
The preparation method of the hard piezoelectric ceramic material provided by the embodiment has the following specific technical scheme:
respectively weighing 100kgPb by using an electronic balance3O4Powder, 15.5kgZrO2Powder, 23.5kg TiO2Powder, 4kgBi2O3Powder, 2kgSb2O3And 5kg of rare earth powder, adding Pb3O4、ZrO2、TiO2、Bi2O3、Sb2O3Pouring the raw material of the rare earth powder into a stirring mill, mixing the raw material with deionized water as a mixed medium and zirconia balls as a ball milling medium for 5 hours by using the stirring mill, controlling the particle size of the powder to be 1-3 mu m, taking out the first mixed slurry, pumping the first mixed slurry into a filter press for filter pressingDewatering, placing the dewatered slurry in a drying oven, and briquetting the slurry at 170 deg.C under a pressure of 0.8 ton/cm2And drying and briquetting. And then, the dried slurry is subjected to open presintering, the presintering temperature is controlled at 850 ℃, and the presintering heat preservation time is 4 hours. Putting the pre-sintered material blocks into a stirring mill for secondary mixing, wherein the ball milling time is 5 hours, then putting the slurry into a sand mill, circulating for 5 times, controlling the particle size of the powder to be 0.6-0.8 mu m, adding 9% of PVA and 1% of surfactant into the obtained second mixed slurry, stirring and placing the second mixed slurry into a storage barrel, controlling the temperature of the slurry entering a spray tower to be 230-250 ℃, discharging the slurry to be 80-100 ℃, and performing spray granulation. Dry pressing and molding the granulated powder, keeping the temperature for 2h at 600 ℃ to remove glue to obtain a molded blank, sealing the molded blank in an alumina crucible, sintering the sealed blank in a program temperature control box furnace at the sintering temperature of 1290 ℃ for 4h to obtain a ceramic wafer with the outer diameter of 20mm, grinding the ceramic wafer to the thickness of 1.5mm, cleaning, applying electrodes on two surfaces, infiltrating silver at the sintering temperature of 800 ℃/10min, polarizing the ceramic wafer (the polarizing medium is air, the polarizing temperature is 200 ℃, the polarizing voltage is 1000V/mm, and maintaining the pressure for 30min), stabilizing for 3 days after polarization, and testing the piezoelectric performance of the ceramic wafer to obtain a product K.
The preparation method is adopted, the difference is only that the sintering temperature is 1330 ℃, and the product L is obtained.
The preparation method is adopted, the difference is that the sintering temperature is 1260 ℃, and the product M is obtained.
Example 3
The preparation method of the hard piezoelectric ceramic material provided by the embodiment has the following specific technical scheme:
respectively weighing 102kgPb by using an electronic balance3O4Powder, 15kgZrO2Powder, 23kg TiO2Powder, 4.5kgBi2O3Powder, 2kgSb2O3And 3.5kg of rare earth powder prepared by mixing Pb3O4、ZrO2、TiO2、Bi2O3、Sb2O3Pouring the raw material of rare earth powder into a stirring mill, using deionized water as a mixing medium, and adding oxygenZirconium balls are used as ball milling media, a stirring mill is used for mixing materials for 5 hours, the particle size of powder is controlled to be 1-3 mu m, the first mixed slurry is taken out, the first mixed slurry is injected into a filter press for pressure filtration and dehydration, the dehydrated slurry is put into a drying box, the slurry is pressed into blocks at the temperature of 170 ℃, and the briquetting pressure is 0.8 ton/cm2And drying and briquetting. And then, the dried slurry is subjected to open presintering, the presintering temperature is controlled at 850 ℃, and the presintering heat preservation time is 4 hours. Putting the pre-sintered material blocks into a stirring mill for secondary ball milling, wherein the ball milling time is 5H, then putting the slurry into a sand mill, circulating for 5 times, controlling the particle size of the powder to be 0.6-0.8 mu m, adding 9% of PVA and 1% of surfactant into the obtained slurry, stirring, putting the obtained mixture into a storage barrel, controlling the temperature of the slurry entering a spray tower, and performing spray granulation. Dry pressing and molding the granulated powder, keeping the temperature at 800 ℃ for 1h for binder removal to obtain a molded blank, sealing the molded blank in an alumina crucible, sintering the sealed blank in a program temperature control box furnace at the sintering temperature of 1290 ℃ for 4h to obtain a ceramic wafer with the outer diameter of 20mm, grinding the ceramic wafer to the thickness of 1.5mm, cleaning, applying electrodes on two surfaces, infiltrating silver at the sintering temperature of 1290 ℃ for 10min, polarizing the ceramic wafer (the polarizing medium is air, the polarizing temperature is 200 ℃, the polarizing voltage is 1000V/mm, and maintaining the pressure for 30min), stabilizing for 3 days after polarization, and testing the piezoelectric performance of the ceramic wafer to obtain a product N.
The preparation method is adopted, the difference is only that the sintering temperature is 1330 ℃, and the product O is obtained.
The preparation method is adopted, the difference is that the sintering temperature is 1260 ℃, and the product P is obtained.
The piezoelectric properties of the hard piezoceramic material products manufactured in 3 examples were tested, and as shown in tables 1 to 3, the formulation of example 1 has the best piezoelectric properties when the sintering temperature is 1290 ℃ and the pre-sintering temperature is 850 ℃, that is, the piezoelectric property of product B is the best, the piezoelectric constant D33 is as high as 415pC/N, the dielectric constant is as high as 1905, the electromechanical coupling coefficient Kp is as high as 0.663, and the mechanical quality factor Qm is 1319.
Table 1 sintering temperature 1290 ℃ test temperature: humidity test at 25 ℃: 40 percent of
Table 2 sintering temperature 1330 ℃ test temperature: humidity test at 25 ℃: 40 percent of
Table 3 sintering temperature 1260 ℃ test temperature: humidity test at 25 ℃: 40 percent of
As shown in FIG. 2-3, the crystal grains of the product B are 9-28 μm, as shown in FIG. 4-5, the crystal grains of the product E are 8-29 μm, and as shown in FIG. 6-7, the crystal grains of the product H are 1-7 μm.
Example 4
The preparation method of the hard piezoelectric ceramic material provided by the embodiment has the following specific technical scheme:
respectively weighing 62kgPb by using an electronic balance3O4Powder, 13kgZrO2Powder, 16kg TiO2Powder, 3.5kgBi2O3Powder, 1.5kgSb2O3And 4kg of rare earth powder prepared by mixing Pb3O4、ZrO2、TiO2、Bi2O3、Sb2O3Pouring the raw material of the rare earth powder into a stirring mill, taking deionized water as a mixed medium, taking zirconia balls as a ball milling medium, mixing materials for 5 hours by using the stirring mill, controlling the particle size of the powder to be 1-3 mu m, taking out first mixed slurry, pumping the first mixed slurry into a filter press for pressure filtration and dehydration, putting the dehydrated slurry into a drying box, pressing the slurry into blocks at the temperature of 170 ℃ and the pressure of 0.8 ton/cm2And drying and briquetting. And then, the dried slurry is subjected to open presintering, the presintering temperature is controlled at 850 ℃, and the presintering heat preservation time is 4 hours. Putting the pre-sintered material blocks into a stirring mill for secondary ball milling for 5H, and then driving the slurry into a sand millCirculating for 5 times in the machine, controlling the particle size of the powder to be 0.6-0.8 mu m, adding 9% of PVA and 1% of surfactant into the obtained slurry, stirring, placing the mixture into a storage barrel, controlling the temperature of the slurry entering a spray tower, and performing spray granulation. Dry pressing and molding the granulated powder, keeping the temperature at 800 ℃ for 1h for binder removal to obtain a molded blank, sealing the molded blank in an alumina crucible, sintering the aluminum crucible in a program temperature control box furnace at 1250 ℃ for 5h to obtain a ceramic wafer with the outer diameter of 20mm, grinding the ceramic wafer to the thickness of 1.5mm, cleaning, applying electrodes on two surfaces, infiltrating silver at the temperature of 800 ℃/10min, polarizing the ceramic wafer (the polarizing medium is air, the polarizing temperature is 200 ℃, the polarizing voltage is 1000V/mm, and maintaining the pressure for 30min), stabilizing for 3 days after polarization, and testing the piezoelectric performance.
Example 5
The preparation method of the hard piezoelectric ceramic material provided by the embodiment has the following specific technical scheme:
respectively weighing 68kgPb by an electronic balance3O4Powder, 13kgZrO2Powder, 15kg TiO2Powder, 1.5kgBi2O3Powder, 0.5kgSb2O3And 2kg of rare earth powder prepared by mixing Pb3O4、ZrO2、TiO2、Bi2O3、Sb2O3Pouring the raw material of the rare earth powder into a stirring mill, taking deionized water as a mixed medium, taking zirconia balls as a ball milling medium, mixing materials for 5 hours by using the stirring mill, controlling the particle size of the powder to be 1-3 mu m, taking out first mixed slurry, pumping the first mixed slurry into a filter press for pressure filtration and dehydration, putting the dehydrated slurry into a drying box, pressing the slurry into blocks at the temperature of 170 ℃ and the pressure of 0.8 ton/cm2And drying and briquetting. And then, the dried slurry is subjected to open presintering, the presintering temperature is controlled at 850 ℃, and the presintering heat preservation time is 4 hours. Putting the pre-sintered material blocks into a stirring mill for secondary ball milling for 5H, then putting the slurry into a sand mill, circulating for 5 times, controlling the particle size of the powder to be 0.6-0.8 mu m, adding 9% of PVA and 1% of surfactant into the obtained slurry, stirring and placing the mixture into a storage barrel, and controlling the mixture to enter a spraying and spraying modeAnd (4) carrying out spray granulation at the slurry temperature in the spray tower. Dry pressing the granulated powder, keeping the temperature at 800 ℃ for 1h for binder removal to obtain a formed blank, sealing the formed blank in an alumina crucible, sintering the sealed blank in a program temperature control box furnace at 1350 ℃ for 3h to obtain a ceramic wafer with the outer diameter of 20mm, grinding the ceramic wafer to the thickness of 1.5mm, cleaning, applying electrodes on two surfaces, infiltrating silver at 800 ℃/10min, polarizing the ceramic wafer (the polarizing medium is air, the polarizing temperature is 200 ℃, the polarizing voltage is 1000V/mm, and maintaining the pressure for 30min), stabilizing for 3 days after polarization, and testing the piezoelectric performance.
The above description is only for the purpose of illustrating preferred embodiments of the present invention and is not to be construed as limiting the invention, and the present invention is not limited to the above examples, and those skilled in the art should also be able to make various changes, modifications, additions or substitutions within the spirit and scope of the present invention.
Claims (10)
1. The preparation method of the hard piezoelectric ceramic material is characterized by comprising the following steps:
s1, weighing the following raw materials in percentage by weight: 62-68% of lead tetraoxide, 10-13% of zirconium dioxide, 15-17% of titanium dioxide, 1.5-3.5% of bismuth trioxide, 0.5-1.5% of antimony trioxide and 2-4% of rare earth, mixing the raw materials for the first time to obtain a first mixed slurry, and performing filter pressing dehydration, drying and briquetting and presintering synthesis treatment to obtain a material block;
s2, performing secondary material mixing on the blocks subjected to pre-sintering synthesis in the step S1 to obtain second mixed slurry, performing spray granulation on the second mixed slurry to obtain powder, and performing molding treatment on the powder to obtain a blank;
s3, performing plastic removal and sintering treatment on the blank in the step S2 to obtain a ceramic blank sheet;
s4, subjecting the ceramic blank sheet in the step S3 to silver electrode and air polarization treatment to obtain the hard piezoelectric ceramic material.
2. The method for preparing a hard piezoceramic material according to claim 1, wherein in the step S1, the first mixing is performed by adding deionized water into a stirring mill to mix and grind various raw materials into slurry with a particle size of 1-3 μm.
3. The method for preparing a hard piezoceramic material according to claim 1, wherein in the step S1, the drying temperature is 170 ℃ and the briquetting pressure is 0.8 ton/cm in the drying briquetting treatment2The temperature of the pre-sintering synthesis is 800-900 ℃, and the time is 3-5 h.
4. The method for preparing a hard piezoelectric ceramic material according to claim 1, wherein in step S2, the second mixing process is to add deionized water into the pre-sintered material block by a stirring mill to grind the material block into slurry with a particle size of 1-3 μm, and then to grind the obtained slurry into slurry with a particle size of 0.6-0.8 μm in a sand mill to obtain a second mixed slurry; the dry pressure of the dry pressing molding treatment is 2.3 tons/cm2。
5. The method for preparing a hard piezoceramic material according to claim 1, wherein in step S2, the spray granulation processing steps are as follows: and adding 9% of polyvinyl alcohol solution and 1% of surfactant into the second mixed slurry, and then sending the mixture into a spray tower for spray granulation treatment.
6. The method for preparing a hard piezoceramic material according to claim 5, wherein the feeding temperature of the spray tower is 230-250 ℃, and the discharging temperature is 80-100 ℃.
7. The method for preparing a hard piezoceramic material according to claim 1, wherein in the step S3, the plastic removal treatment is to heat the blank to 600-800 ℃ and keep the temperature for 2-3 h.
8. The method for preparing a hard piezoceramic material according to claim 1, wherein in step S3, an alumina crucible is used for sintering treatment, the sintering treatment temperature is 1250-1350 ℃, and the sintering time is 3-5 h.
9. The method for preparing a hard piezoelectric ceramic material according to claim 1, wherein in step S4, before being treated by the silver electrode, the ceramic green sheet is subjected to size processing and ultrasonic cleaning, the silver electrode treatment is carried out by subjecting the ceramic green sheet after size processing to silver coating on the upper surface and the lower surface, the silver firing temperature is 750-850 ℃, and the silver impregnation is 800 ℃/10 min.
10. The method for preparing a hard piezoelectric ceramic material according to claim 1, wherein in step S4, the air polarization treatment is to polarize the ceramic green sheet processed by the silver electrode in air at 200 ℃, the polarization voltage is 1000V/mm, and the pressure is maintained for 30 min.
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