CN114644524A - High-performance lithium-calcium-tantalum-nickel-zinc-niobium-magnesium-tungsten modified PZT piezoelectric ceramic prepared at low temperature - Google Patents
High-performance lithium-calcium-tantalum-nickel-zinc-niobium-magnesium-tungsten modified PZT piezoelectric ceramic prepared at low temperature Download PDFInfo
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Abstract
The invention discloses a high-performance PZT piezoelectric ceramic material modified by lithium-calcium-tantalum-nickel-zinc-niobium-magnesium-tungsten prepared at low temperature and a preparation method thereof, wherein the general formula of the piezoelectric ceramic is Pb1‑x‑yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1‑u‑v‑wO3Expressed that x is more than or equal to 0.001 and less than or equal to 0.005, y is more than or equal to 0.001 and less than or equal to 0.005, u is more than or equal to 0 and less than or equal to 0.005, v is more than or equal to 0.01 and less than or equal to 0.05, and w is more than or equal to 0.01 and less than or equal to 0.05. Preparing PZT modified piezoelectric ceramic powder sintered at the low temperature of 850-950 ℃ by adopting a solid-phase reaction method, and preparing a ceramic material by processes of granulation, tabletting, binder removal, sintering, silver firing, polarization and the like. The result shows that the PZT modified ceramic material is prepared at the sintering temperature of 850-950 ℃, the crystal grains are compact, the crystal grains are uniform and are fully crystallized, the liquid phase sintering characteristic is obvious, and the piezoelectric property is greatly improved.
Description
Technical Field
The invention belongs to the field of piezoelectric ceramic materials, and particularly relates to a high-performance lithium-calcium-tantalum-nickel-zinc-niobium-magnesium-tungsten modified PZT piezoelectric ceramic prepared at a low temperature.
Background
PZT is traditional piezoelectric ceramics, has good effects of dielectric, ferroelectric, piezoelectric, pyroelectric and the like, has low raw material price, is suitable for factory production, and can be modified to obtain ceramic materials suitable for multiple purposes. The multilayer piezoelectric ceramic has alternating ceramic layers and internal metal electrode layers. With the rapid development of science and technology, multilayer piezoelectric ceramics are widely researched and widely applied to brakes, converters and sensors. The Ag-Pd electrode is generally used as an inner electrode of multilayer ceramic, the co-firing temperature range is 920-980 ℃, and the sintering temperature of the pure Ag inner electrode is not required to be higher than 900 ℃. The conventional PZT modified piezoelectric ceramic is sintered at a high temperature of about 1200 deg.c, so that the internal electrodes cannot use pure Ag (melting point ≈ 961 deg.c) at such a high temperature, and the Ag — Pd electrode layer also diffuses to the ceramic layer, resulting in deterioration of electrical properties of the ceramic, thereby affecting the reliability of the multilayer device.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and the first aim of the invention is to provide a formula of a high-performance PZT modified piezoelectric ceramic material prepared at low temperature, wherein the piezoelectric ceramic material has low sintering temperature and good piezoelectric performance; the second purpose of the invention is to provide a preparation method of the high-performance PZT modified piezoelectric ceramic prepared at low temperature, so as to reduce the sintering temperature of the PZT modified piezoelectric ceramic and improve the piezoelectric performance.
Aiming at the first object of the invention, the invention provides a high-performance PZT modified piezoelectric ceramic prepared at low temperature, and the chemical formula of the piezoelectric ceramic is Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v- wO3Expressed that x is more than or equal to 0.001 and less than or equal to 0.005, y is more than or equal to 0.001 and less than or equal to 0.005, u is more than or equal to 0 and less than or equal to 0.005, v is more than or equal to 0.01 and less than or equal to 0.05, and w is more than or equal to 0.01 and less than or equal to 0.05.
Aiming at the second invention purpose of the invention, a plurality of elements Ta, Li, Ca, Ni, Zn, W, Mg and Nb are introduced into the PZT modified piezoelectric ceramic to enter A or B position, and the PZT modified piezoelectric ceramic with good piezoelectric property is prepared at the sintering temperature of 850-950 ℃, and the specific process steps are as follows:
(1) preparation of PZT modified ceramic powder
According to the general formula Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v-wO3Expressed as x is more than or equal to 0.001 and less than or equal to 0.005, y is more than or equal to 0.001 and less than or equal to 0.005, u is more than or equal to 0 and less than or equal to 0.005, v is more than or equal to 0.01 and less than or equal to 0.05, and w is more than or equal to 0.01 and less than or equal to 0.05, the raw materials are calculated and weighed, crushed by ball milling and mixedAfter uniform mixing, keeping the temperature at 750-850 ℃ for 2-4 h, cooling to room temperature after heat preservation, and performing ball milling and crushing again to obtain PZT modified ceramic powder;
(2) granulating and tabletting
Adding 5-10 wt% of polyvinyl alcohol solution into the PZT modified ceramic powder obtained in the step (1) for granulation, and then pressing the obtained granules into tablets to obtain the PZT modified ceramic wafer;
(3) binder removal sintering
Removing glue from the PZT modified piezoelectric ceramic piece obtained in the step (2), and then sintering at 850-950 ℃ for 2-4 h in a heat preservation manner to obtain a sintered PZT modified piezoelectric ceramic piece;
(4) polarization of
And (3) coating 5-15 wt% of silver paste on the surface of the sintered PZT modified piezoelectric ceramic wafer obtained in the step (3), then carrying out heat preservation sintering at 650-750 ℃ for 10-20 min, cooling to room temperature after heat preservation is finished, and then carrying out polarization in silicone oil to obtain the high-performance PZT modified piezoelectric ceramic.
In the above method, the specific process of the two ball milling in step (1) is preferably: the method comprises the steps of taking absolute ethyl alcohol as a dispersion medium, adding the raw materials and the absolute ethyl alcohol into a ball milling tank according to the mass ratio of the total amount of the raw materials to the absolute ethyl alcohol of 1:1.5, carrying out ball milling on a planetary ball mill for 10-24 hours at the rotating speed of 100-450 rmp, and drying after ball milling. The drying may be baking under a baking lamp for 2 to 3 hours.
In the above method, the specific process for compressing the obtained pellets into tablets is preferably: and pressing the mixture into a high-performance PZT modified piezoelectric ceramic piece with the diameter of about 10-15 mm and the thickness of about 0.8-1.2 mm under the pressure of 10-20 MPa.
In the above method, the concentration of the polyvinyl alcohol solution in the step (2) is preferably 5 to 10 wt%.
In the above method, the specific process of discharging the glue in the step (3) is preferably: and (3) preserving the heat of the PZT modified ceramic wafer obtained in the step (2) for 4-10 h at the temperature of 450-550 ℃.
In the method, the specific process for polarizing in the silicone oil in the step (4) is as follows: keeping the electric field intensity for 15-30 min under the condition that the polarization field intensity is 2-5 kV/mm in silicone oil at the temperature of 60-120 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. the high-performance PZT modified piezoelectric ceramic provided by the invention has low sintering temperature of 850-950 ℃ and good piezoelectric performance, and d33Up to 640pC/N, a dielectric loss of not more than three thousandths measured at room temperature at a frequency of 1kHz using an agilent 4294A precision impedance apparatus, and a curie temperature of more than 299 ℃, as shown in fig. 3.
2. The phase of the high-performance PZT modified piezoelectric ceramic prepared at low temperature is a pure perovskite phase, as shown in figure 1, and the added Ta, Li, Ca, Ni, Zn, W, Mg and Nb elements improve the sintering activity, so that the crystal grains are compact, uniform, fully grown and compact.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of the piezoelectric ceramic material prepared in examples 1 to 6.
FIG. 2 is a graph showing the piezoelectric properties of the piezoelectric ceramic materials prepared in examples 1 to 6.
FIG. 3 shows the change of dielectric constant with temperature of the piezoelectric ceramic materials prepared in examples 1 to 6.
FIG. 4 is a schematic view of an electroacoustic device, which is a piezoelectric ceramic material prepared in example 2.
Detailed Description
The high-performance PZT modified piezoelectric ceramics prepared at low temperature according to the present invention will be further described by the following embodiments.
Example 1
(1) Preparation of PZT modified ceramic powder
According to the general formula Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v-wO3The raw materials are weighed by calculation, (x is 0.001, y is 0.001, u is 0, v is 0.01, w is 0.01), the raw materials and the absolute ethyl alcohol are added into a ball milling tank according to the mass ratio of the total amount of the raw materials to the absolute ethyl alcohol of 1:1.5 by taking the absolute ethyl alcohol as a dispersion medium, the raw materials and the absolute ethyl alcohol are ball milled for 24 hours on a planetary ball mill at the rotating speed of 100rmp, the ball milled raw materials are baked for 2 hours under a baking lamp to obtain mixed powder, and the mixed powder is dried after being ball milled, so that the mixed powder is obtainedKeeping the temperature of the obtained mixed powder at 800 ℃ for 3h, cooling to room temperature after heat preservation, performing secondary ball milling according to the same method again, baking for 3h under a baking lamp after ball milling, and drying to obtain PZT modified ceramic powder;
(2) granulating and tabletting
Adding 10 wt% polyvinyl alcohol solution into the PZT modified ceramic powder obtained in the step (1) for granulation, and then pressing under the pressure of 10MPa to obtain a PZT modified piezoelectric ceramic wafer with the diameter of about 10mm and the thickness of about 1.2 mm;
(3) binder removal sintering
Keeping the PZT modified ceramic wafer obtained in the step (2) at 550 ℃ for 4h for glue removal, and then keeping the temperature at 850 ℃ for sintering for 4h to obtain a sintered PZT modified piezoelectric ceramic wafer;
(4) polarization of
And (4) coating silver paste with the weight percent of 10% on the surface of the sintered PZT modified piezoelectric ceramic wafer obtained in the step (3), carrying out heat preservation sintering at 650 ℃ for 20min, cooling to room temperature after heat preservation, and then, in silicone oil at 120 ℃, keeping the electric field strength for 15min under the condition that the polarization field strength is 3kV/mm, and polarizing to obtain the high-performance PZT modified piezoelectric ceramic prepared at low temperature.
The XRD pattern of the prepared high-performance PZT modified piezoelectric ceramic prepared at low temperature is shown in figure 1, and figure 1 shows that the PZT modified piezoelectric ceramic is a pure perovskite phase; quasi-static d of ZJ-3 type using the Acoustic institute of Chinese academy of sciences33Meter, measured piezoelectric coefficient d33See FIG. 2, 570 pC/N; the change of the dielectric constant with the temperature is measured by connecting an Agilent 4980A precision impedance instrument with a temperature control furnace, and the Curie temperature of the sample is 307 ℃ as can be obtained from the graph shown in FIG. 3.
Example 2
(1) Preparation of PZT modified ceramic powder
According to the general formula Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v-wO3The respective raw materials were weighed out and calculated (x ═ 0.0015, y ═ 0.0015, u ═ 0.001, v ═ 0.03, and w ═ 0.015), and anhydrous ethanol was used as a dispersion medium, and the mass ratio of the total amount of the respective raw materials to the anhydrous ethanol was 1:1.5Adding absolute ethyl alcohol into a ball milling tank, ball milling for 10 hours on a planetary ball mill at the rotating speed of 450rmp, baking for 3 hours after ball milling to obtain mixed powder, preserving the temperature of the obtained mixed powder for 4 hours at 750 ℃, cooling to room temperature after heat preservation, performing secondary ball milling according to the same method again, baking for 3 hours after ball milling to obtain PZT modified ceramic powder;
(2) granulating and tabletting
Adding 8 wt% polyvinyl alcohol solution into the PZT modified ceramic powder obtained in the step (1) for granulation, and then pressing under the pressure of 20MPa to obtain a PZT modified piezoelectric ceramic wafer with the diameter of about 14mm and the thickness of about 0.9 mm;
(3) binder removal sintering
Preserving heat of the PZT modified piezoelectric ceramic piece obtained in the step (2) at 550 ℃ for 4h for glue removal, and then preserving heat and sintering at 900 ℃ for 3h to obtain a sintered PZT modified piezoelectric ceramic piece;
(4) polarization of
And (4) coating 12 wt% of silver paste on the surface of the sintered PZT modified piezoelectric ceramic wafer obtained in the step (3), carrying out heat preservation sintering at 700 ℃ for 10min, cooling to room temperature after heat preservation, and then, in 120 ℃ silicone oil, keeping the electric field strength for 30min under the condition that the polarization field strength is 3kV/mm, and polarizing to obtain the high-performance PZT modified piezoelectric ceramic prepared at low temperature.
The XRD pattern of the prepared high-performance PZT modified piezoelectric ceramic prepared at low temperature is shown in figure 1, and figure 1 shows that the PZT modified piezoelectric ceramic is a pure perovskite phase; quasi-static d of ZJ-3 type using the Acoustic institute of Chinese academy of sciences33Meter, measured piezoelectric coefficient d33FIG. 2, 580 pC/N; the change of the dielectric constant with the temperature is measured by connecting an Agilent 4980A precision impedance instrument with a temperature control furnace, and the Curie temperature of the sample is 305 ℃ as can be obtained from the graph shown in FIG. 3.
Example 3
(1) Preparation of PZT modified ceramic powder
According to the general formula Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v-wO3Denotes that (x ═ 0.002, y ═ 0.002, u ═ 0.003, and v ═ 0.0030.05, w is 0.02), adding the raw materials and absolute ethyl alcohol into a ball milling tank by taking absolute ethyl alcohol as a dispersion medium, adding the raw materials and the absolute ethyl alcohol into the ball milling tank according to the mass ratio of the total amount of the raw materials to the absolute ethyl alcohol of 1:1.5, carrying out ball milling on a planet ball mill for 18 hours at the rotating speed of 300rmp, baking the ball milled powder for 3 hours under a baking lamp to dry the ball milled powder to obtain mixed powder, keeping the temperature of the obtained mixed powder at 850 ℃ for 2 hours, cooling the obtained mixed powder to room temperature after the heat preservation is finished, carrying out secondary ball milling according to the same method again, baking the ball milled powder under the baking lamp for 2 hours to dry the mixed powder to obtain PZT modified ceramic powder;
(2) granulating and tabletting
Adding 10 wt% polyvinyl alcohol solution into the PZT modified ceramic powder obtained in the step (1) for granulation, and then pressing under the pressure of 15MPa to obtain a PZT modified piezoelectric ceramic wafer with the diameter of about 13mm and the thickness of about 1 mm;
(3) binder removal sintering
Preserving the heat of the PZT modified piezoelectric ceramic piece obtained in the step (2) at 450 ℃ for 10h for glue removal, and then preserving the heat of the PZT modified piezoelectric ceramic piece at 950 ℃ for 2h for sintering to obtain a sintered PZT modified piezoelectric ceramic piece;
(4) polarization of
And (3) coating 5 wt% of silver paste on the surface of the sintered PZT modified piezoelectric ceramic wafer obtained in the step (3), carrying out heat preservation sintering at 750 ℃ for 10min, cooling to room temperature after heat preservation, and then keeping the electric field intensity for 16min in silicone oil at 120 ℃ under the condition that the polarization field intensity is 3kV/mm for polarization to obtain the high-performance PZT modified piezoelectric ceramic prepared at low temperature.
The XRD pattern of the prepared high-performance PZT modified piezoelectric ceramic prepared at low temperature is shown in figure 1, and figure 1 shows that the PZT modified piezoelectric ceramic is a pure perovskite phase; quasi-static d of ZJ-3 type using the Acoustic institute of Chinese academy of sciences33Meter, measured piezoelectric coefficient d33See FIG. 2, at 590 pC/N; the change of the dielectric constant with the temperature is measured by connecting an Agilent 4980A precision impedance instrument with a temperature control furnace, and the Curie temperature of the sample is 301 ℃ as can be obtained from the graph shown in FIG. 3.
Example 4
(1) Preparation of PZT modified ceramic powder
According to the general formula Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v-wO3Calculating and weighing raw materials, (x is 0.0025, y is 0.0025, u is 0.005, v is 0.07, and w is 0.025), adding the raw materials and absolute ethyl alcohol into a ball milling tank according to the mass ratio of the total amount of the raw materials to the absolute ethyl alcohol of 1:1.5, carrying out ball milling on the raw materials for 20 hours at the rotating speed of 200rmp on a planetary ball mill, baking the raw materials for 3 hours after ball milling to obtain mixed powder, keeping the temperature of the mixed powder at 800 ℃ for 3 hours, cooling the mixed powder to room temperature after heat preservation, carrying out secondary ball milling according to the same method again, baking the mixed powder for 3 hours after ball milling to obtain PZT modified ceramic powder;
(2) granulating and tabletting
Adding 10 wt% polyvinyl alcohol solution into the PZT modified ceramic powder obtained in the step (1) for granulation, and then pressing under the pressure of 20MPa to obtain a PZT modified piezoelectric ceramic wafer with the diameter of about 15mm and the thickness of about 0.8 mm;
(3) binder removal sintering
Keeping the PZT modified piezoelectric ceramic sheet obtained in the step (2) at 500 ℃ for 8h for glue removal, and then keeping the temperature at 900 ℃ for sintering for 4h to obtain a sintered PZT modified piezoelectric ceramic sheet;
(4) polarization of
And (3) coating silver paste with the weight percent of 15% on the surface of the sintered PZT modified piezoelectric ceramic wafer obtained in the step (3), carrying out heat preservation sintering at 650 ℃ for 15min, cooling to room temperature after heat preservation, and then keeping the electric field intensity for 25min in silicone oil with the temperature of 120 ℃ and the polarization field intensity of 3kV/mm for polarization to obtain the high-performance PZT modified piezoelectric ceramic prepared at low temperature.
The XRD pattern of the prepared high-performance PZT modified piezoelectric ceramic prepared at low temperature is shown in figure 1, and figure 1 shows that the PZT modified piezoelectric ceramic is a pure perovskite phase; quasi-static d of ZJ-3 type using the Acoustic institute of Chinese academy of sciences33Meter, measured piezoelectric coefficient d33See FIG. 2, 595 pC/N; the change of the dielectric constant with the temperature is measured by connecting an Agilent 4980A precision impedance instrument with a temperature control furnace, and the Curie temperature of the sample is 306 ℃ as shown in figure 3.
Example 5
(1) Preparation of PZT modified ceramic powder
According to the general formula Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v-wO3Calculating and weighing raw materials, (x is 0.003, y is 0.003, u is 0.007, v is 0.08, and w is 0.03), adding the raw materials and absolute ethyl alcohol into a ball milling tank according to the mass ratio of the total amount of the raw materials to the absolute ethyl alcohol of 1:1.5 by using the absolute ethyl alcohol as a dispersion medium, carrying out ball milling on a planetary ball mill at the rotating speed of 400rmp for 11 hours, baking under a baking lamp for 2 hours after ball milling to obtain mixed powder, carrying out heat preservation on the obtained mixed powder at 750 ℃ for 4 hours, cooling to room temperature after heat preservation, carrying out secondary ball milling according to the same method again, baking under the baking lamp for 3 hours after ball milling to obtain PZT modified ceramic powder;
(2) granulating and tabletting
Adding a polyvinyl alcohol solution with the concentration of 6 wt% into the PZT modified ceramic powder obtained in the step (1) for granulation, and then pressing the mixture into a PZT modified piezoelectric ceramic wafer with the diameter of about 10mm and the thickness of about 1.2mm under the pressure of 18 MPa;
(3) binder removal sintering
Keeping the PZT modified piezoelectric ceramic sheet obtained in the step (2) at 500 ℃ for 7h for glue removal, and then keeping the temperature at 900 ℃ for sintering for 4h to obtain a sintered PZT modified piezoelectric ceramic sheet;
(4) polarization of
And (3) coating silver paste with the weight percent of 10% on the surface of the sintered PZT modified piezoelectric ceramic wafer obtained in the step (3), carrying out heat preservation sintering at 750 ℃ for 12min, cooling to room temperature after heat preservation, and then keeping the electric field intensity for 30min in silicone oil with the temperature of 120 ℃ and the polarization field intensity of 3kV/mm for polarization to obtain the high-performance PZT modified piezoelectric ceramic prepared at low temperature.
The XRD pattern of the prepared high-performance PZT modified piezoelectric ceramic prepared at low temperature is shown in figure 1, and figure 1 shows that the PZT modified piezoelectric ceramic is a pure perovskite phase; quasi-static d of ZJ-3 type using the Acoustic institute of Chinese academy of sciences33Meter, measured piezoelectric coefficient d33See FIG. 2, 640 pC/N; the change of the dielectric constant with the temperature is measured by connecting an Agilent 4980A precise impedance instrument with a temperature control furnace, and a sample can be obtained from the graph shown in FIG. 3The Curie temperature of (A) was 303 ℃.
Example 6
(1) Preparation of PZT modified ceramic powder
According to the general formula Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v-wO3Weighing raw materials, (x ═ 0.0035, y ═ 0.0035, u ═ 0.009, v ═ 0.09, and w ═ 0.035), adding the raw materials and absolute ethyl alcohol into a ball milling tank according to the mass ratio of the total amount of the raw materials to the absolute ethyl alcohol of 1:1.5, carrying out ball milling on a planetary ball mill at the rotating speed of 100rmp for 24 hours, baking under a baking lamp after ball milling for 2 hours to obtain mixed powder, keeping the temperature of the obtained mixed powder at 800 ℃ for 3 hours, cooling to room temperature after heat preservation, carrying out secondary ball milling according to the same method again, baking under the baking lamp after ball milling for 3 hours to obtain PZT modified ceramic powder;
(2) granulating and tabletting
Adding 10 wt% polyvinyl alcohol solution into the PZT modified ceramic powder obtained in the step (1) for granulation, and then pressing under the pressure of 10MPa to obtain a PZT modified piezoelectric ceramic wafer with the diameter of about 10mm and the thickness of about 1.2 mm;
(3) binder removal sintering
Keeping the PZT modified piezoelectric ceramic sheet obtained in the step (2) at 550 ℃ for 4h for glue removal, and then keeping the temperature at 850 ℃ for sintering for 4h to obtain a sintered PZT modified piezoelectric ceramic sheet;
(4) polarization of
And (3) coating silver paste with the weight percent of 10% on the surface of the sintered PZT modified piezoelectric ceramic wafer obtained in the step (3), carrying out heat preservation sintering at 650 ℃ for 20min, cooling to room temperature after heat preservation, and then keeping the electric field intensity for 15min in silicone oil with the temperature of 120 ℃ and the polarization field intensity of 3kV/mm for polarization to obtain the high-performance PZT modified piezoelectric ceramic prepared at low temperature.
The XRD pattern of the prepared high-performance PZT modified piezoelectric ceramic prepared at low temperature is shown in figure 1, and figure 1 shows that the PZT modified piezoelectric ceramic is a pure perovskite phase; quasi-static d of ZJ-3 type using the Acoustic institute of Chinese academy of sciences33Meter, measured piezoelectric coefficient d33See FIG. 2, 570 pC/N; the change of the dielectric constant with the temperature is measured by connecting an Agilent 4980A precise impedance instrument with a temperature control furnace, and the Curie temperature of the sample is 299 ℃ which can be obtained from the graph shown in FIG. 3.
Example 7
(1) Preparation of PZT modified ceramic powder
According to the general formula Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v-wO3Calculating and weighing the raw materials, (x is 0.004, y is 0.004, u is 0.002, v is 0.02 and w is 0.04), adding the raw materials and absolute ethyl alcohol into a ball milling tank according to the mass ratio of the total amount of the raw materials to the absolute ethyl alcohol of 1:1.5 by using the absolute ethyl alcohol as a dispersion medium, carrying out ball milling on the raw materials for 24 hours at the rotating speed of 100rmp on a planet ball mill, baking the raw materials for 2 hours after ball milling to obtain mixed powder, keeping the temperature of the obtained mixed powder at 800 ℃ for 3 hours, cooling the mixed powder to room temperature after the temperature is kept, carrying out secondary ball milling according to the same method again, baking the raw materials for 3 hours after ball milling to obtain PZT modified ceramic powder;
(2) granulating and tabletting
Adding 10 wt% polyvinyl alcohol solution into the PZT modified ceramic powder obtained in the step (1) for granulation, and then pressing under the pressure of 10MPa to obtain a PZT modified piezoelectric ceramic wafer with the diameter of about 10mm and the thickness of about 1.2 mm;
(3) binder removal sintering
Keeping the PZT modified piezoelectric ceramic sheet obtained in the step (2) at 550 ℃ for 4h for glue removal, and then keeping the temperature at 850 ℃ for sintering for 4h to obtain a sintered PZT modified piezoelectric ceramic sheet;
(4) polarization of
And (3) coating silver paste with the weight percent of 10% on the surface of the sintered PZT modified piezoelectric ceramic wafer obtained in the step (3), carrying out heat preservation sintering at 650 ℃ for 20min, cooling to room temperature after heat preservation, and then keeping the electric field intensity for 15min in silicone oil with the temperature of 120 ℃ and the polarization field intensity of 3kV/mm for polarization to obtain the high-performance PZT modified piezoelectric ceramic prepared at low temperature.
Example 8
(1) Preparation of PZT modified ceramic powder
According to the general formula Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v-wO3Calculating and weighing raw materials, (x is 0.0045, y is 0.0045, u is 0.004, v is 0.04, and w is 0.045), adding the raw materials and absolute ethyl alcohol into a ball milling tank according to the mass ratio of the total amount of the raw materials to the absolute ethyl alcohol of 1:1.5, carrying out ball milling on the raw materials for 24 hours at a rotating speed of 100rmp on a planet ball mill, baking the raw materials for 2 hours after ball milling to obtain mixed powder, keeping the temperature of the obtained mixed powder at 800 ℃ for 3 hours, cooling the mixed powder to room temperature after heat preservation, carrying out secondary ball milling according to the same method again, baking the mixed powder for 3 hours after ball milling to obtain PZT modified ceramic powder;
(2) granulating and tabletting
Adding 10 wt% polyvinyl alcohol solution into the PZT modified ceramic powder obtained in the step (1) for granulation, and then pressing under the pressure of 10MPa to obtain a PZT modified piezoelectric ceramic wafer with the diameter of about 10mm and the thickness of about 1.2 mm;
(3) binder removal sintering
Keeping the PZT modified piezoelectric ceramic sheet obtained in the step (2) at 550 ℃ for 4h for glue removal, and then keeping the temperature at 850 ℃ for sintering for 4h to obtain a sintered PZT modified piezoelectric ceramic sheet;
(4) polarization of
Coating silver paste with the weight percent of 10% on the surface of the sintered PZT modified piezoelectric ceramic wafer obtained in the step (3), carrying out heat preservation sintering at 650 ℃ for 20min, cooling to room temperature after heat preservation, and then keeping the electric field intensity for 15min in silicone oil with the temperature of 120 ℃ and the polarization field intensity of 3kV/mm for polarization to obtain the high-performance PZT modified piezoelectric ceramic prepared at the low temperature
Application example 1
The high-performance PZT modified piezoceramic material prepared at low temperature obtained in example 6 was prepared into a wafer having a thickness of 0.2 mm and a diameter of 12 mm, and an electroacoustic device was fabricated by adding electrodes, leads, a diaphragm, a case, and the like, as shown in fig. 4.
Claims (10)
1. Low-temperature preparationThe high-performance lithium-calcium-tantalum-nickel-zinc-niobium-magnesium-tungsten modified PZT piezoelectric ceramic is characterized in that the chemical general formula of the piezoelectric ceramic is Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v-wO3Expressed that x is more than or equal to 0.001 and less than or equal to 0.005, y is more than or equal to 0.001 and less than or equal to 0.005, u is more than or equal to 0 and less than or equal to 0.005, v is more than or equal to 0.01 and less than or equal to 0.05, and w is more than or equal to 0.01 and less than or equal to 0.05.
2. The method for preparing the high-performance PZT modified piezoelectric ceramic according to claim 1, comprising the steps of:
(1) preparation of PZT modified ceramic powder
According to the general formula Pb1-x-yLixCayTau[(Ni,Zn)1/3Nb2/3]v(Mg1/2W1/2)w(Ti,Zr)1-u-v-wO3Expressed as x is more than or equal to 0.001 and less than or equal to 0.005, y is more than or equal to 0.001 and less than or equal to 0.005, u is more than or equal to 0 and less than or equal to 0.005, v is more than or equal to 0.01 and less than or equal to 0.05, w is more than or equal to 0.01 and less than or equal to 0.05, the raw materials are calculated and weighed, are subjected to ball milling crushing and uniformly mixing, are subjected to heat preservation at 750-850 ℃ for 2-4 h, are cooled to room temperature after the heat preservation is finished, and are subjected to ball milling crushing again to obtain PZT modified ceramic powder;
(2) granulating and tabletting
Adding a polyvinyl alcohol solution into the PZT modified ceramic powder obtained in the step (1) for granulation, and then pressing the obtained granules into tablets to obtain a PZT modified ceramic chip;
(3) binder removal sintering
Removing glue from the PZT modified piezoelectric ceramic piece obtained in the step (2), and then sintering at 850-950 ℃ for 2-4 h in a heat preservation manner to obtain a sintered PZT modified piezoelectric ceramic piece;
(4) polarization of
And (3) coating 5-15 wt% of silver paste on the surface of the sintered PZT modified piezoelectric ceramic wafer obtained in the step (3), then carrying out heat preservation sintering at 650-750 ℃ for 10-20 min, cooling to room temperature after heat preservation is finished, and then carrying out polarization in silicone oil to obtain the high-performance PZT modified piezoelectric ceramic prepared at low temperature.
3. The method for preparing the high-performance PZT modified piezoelectric ceramic prepared at low temperature according to claim 2, wherein the specific process of ball milling twice in the step (1) is as follows: the method comprises the steps of taking absolute ethyl alcohol as a dispersion medium, adding the raw materials and the absolute ethyl alcohol into a ball milling tank according to the mass ratio of the total amount of the raw materials to the absolute ethyl alcohol of 1:1.5, carrying out ball milling on a planetary ball mill for 10-24 hours at the rotating speed of 100-450 rmp, and drying after ball milling.
4. The method for preparing a high-performance PZT modified piezoelectric ceramic according to claim 3, wherein the drying is baking under a baking lamp for 2-3 hours.
5. The method for preparing the high-performance PZT modified piezoelectric ceramic prepared at low temperature according to any one of claims 2-4, wherein the specific process for pressing the obtained pellets into tablets in step (2) is as follows: and pressing the mixture into a high-performance PZT modified piezoelectric ceramic sheet with the diameter of about 10-15 mm and the thickness of about 0.8-1.2 mm under the pressure of 10-20 MPa.
6. The method for preparing a high-performance PZT modified piezoelectric ceramic prepared at a low temperature according to any one of claims 2-4, wherein the concentration of the polyvinyl alcohol solution in step (2) is 5-10 wt%.
7. The preparation method of the high-performance PZT modified piezoelectric ceramic prepared at low temperature according to any one of claims 2-4, wherein the concrete process of glue discharging in the step (3) is as follows: and (3) preserving the heat of the PZT modified ceramic wafer obtained in the step (2) for 4-10 h at the temperature of 450-550 ℃.
8. The method for preparing the high-performance PZT modified piezoelectric ceramic prepared at low temperature according to any one of claim 5, wherein the concrete process for removing the gel in the step (3) is as follows: and (3) preserving the heat of the PZT modified ceramic wafer obtained in the step (2) for 4-10 h at the temperature of 450-550 ℃.
9. The preparation method of the high-performance PZT modified piezoelectric ceramic prepared at low temperature according to any one of claims 2-4, wherein the specific process of polarization in silicone oil in the step (4) is as follows: keeping the electric field intensity for 15-30 min under the condition that the polarization field intensity is 2-5 kV/mm in silicone oil at the temperature of 60-120 ℃.
10. The method for preparing high-performance PZT modified piezoelectric ceramics according to any of claims 5, wherein the specific process of polarization in silicone oil in step (4) is as follows: and keeping the electric field intensity for 15-30 min in silicone oil at the temperature of 60-120 ℃ under the condition that the polarization field intensity is 2-5 kV/mm.
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