CN115894020A - PMNZT-based piezoelectric ceramic with high piezoelectric coefficient and preparation method and application thereof - Google Patents
PMNZT-based piezoelectric ceramic with high piezoelectric coefficient and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of piezoelectric ceramics, and discloses PMNZT-based piezoelectric ceramics with high piezoelectric coefficient, and a preparation method and application thereof. The PMNZT-based piezoelectric ceramic with high piezoelectric coefficient is prepared by selecting lead magnesium niobate-lead zirconate-lead titanate ternary ceramic with excellent performance as a substrate, introducing trivalent ions with the radius slightly smaller than that of Pb ions into the A position to cause lattice distortion and enhance the relaxation characteristic of the ceramic, thereby obtaining higher dielectric and piezoelectric properties; the piezoelectric ceramicsPositive piezoelectric coefficient d of porcelain 33 Up to 1040pC/N, inverse piezoelectric coefficient d 33 * Up to 1310pm/V, dielectric constant epsilon 33 4530-6460, dielectric loss tan delta less than 0.03, and planar electromechanical coupling coefficient k p Is more than 0.70, and the preparation process of the piezoelectric ceramic is simple, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of piezoelectric ceramics, and particularly relates to PMNZT-based piezoelectric ceramics with high piezoelectric coefficient, and a preparation method and application thereof.
Background
Piezoelectric ceramics are functional ceramic materials with the function of mutual conversion between mechanical energy and electric energy, and are widely applied to the fields of sensors, drivers, transformers, transducers and the like. In a piezoelectric ceramic system, the most widely used system at present is lead zirconate titanate piezoelectric ceramic, which is a solid solution ceramic material consisting of lead zirconate and lead titanate, and in a commercial piezoelectric ceramic system, the component with excellent piezoelectric performance is PZT5 series ceramic, and the piezoelectric coefficient d of the ceramic is 33 Is 500-800pC/N. With the rapid development of electronic components, the fields of high-precision sensors, drivers and the like put forward higher requirements on the performance of piezoelectric ceramics, high-performance piezoelectric ceramic materials with piezoelectric coefficients larger than 800pC/N are urgently needed, and the traditional lead zirconate titanate ceramics obviously cannot meet the performance requirements on the materials put forward by various application conditions. Therefore, the development of piezoelectric ceramic materials with higher dielectric and piezoelectric properties is a technical problem to be solved by those skilled in the art.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a PMNZT-based piezoelectric ceramic with high piezoelectric coefficient, which has high dielectric and high piezoelectric performance, wherein the piezoelectric coefficient d 33 Up to 1040pC/N, inverse piezoelectric coefficient d 33 * Up to 1310pm/V, dielectric constant epsilon 33 4530-6460, and dielectric loss tan delta less than 0.03.
The first aspect of the invention provides a PMNZT-based piezoelectric ceramic with a high piezoelectric coefficient, which has a chemical general formula as follows: pb (1-y) Ln y (Mg 1/3 Nb 2/3 ) (0.85-x) Zr 0.15 Ti x O 3 Wherein x is more than or equal to 0.31 and less than or equal to 0.34,0.02 and less than or equal to 0.025, x and y both represent mole fractions, and Ln is one or two of Nd and Eu elements.
The PMNZT-based piezoelectric ceramic with high piezoelectric coefficient is based on a PMNZT (lead magnesium niobate-lead zirconate-lead titanate) ternary system, and compared with a binary system, the ternary solid solution system can reduce the free energy of materials, so that the lowest eutectic point is reduced, the sintering temperature is reduced macroscopically, and the PMNZT-based piezoelectric ceramic is beneficial to promoting the sintering and reducing the volatilization of lead ions in the sintering process; meanwhile, the micro-morphology is also beneficial to inhibiting excessive growth of local grains, forming uniform and compact morphology and improving the mechanical strength of the ceramic. In addition, the PMNZT ternary system adopted by the invention can integrate the advantages of each component, has rich adjustability near the morphotropic phase boundary, can obtain the morphotropic phase boundary with the coexistence of a trigonal phase and a tetragonal phase by adjusting the components of the ternary ceramic, has the state of the coexistence of a plurality of ferroelectric domains near the morphotropic phase boundary, has small energy barrier among the plurality of ferroelectric domains, is more beneficial to promoting the polarization turnover of the ferroelectric domains, and thus obtains high dielectric and piezoelectric properties; compared with other ternary system lead-based piezoelectric ceramics, the piezoelectric performance of the ternary system lead-based piezoelectric ceramics after A-site doping is not obviously improved, and the component content change of the ternary system and the concentration of doped ions have great influence on the performance. The invention also introduces trivalent ions with slightly smaller radius than Pb ions at the A position to cause lattice distortion and enhance the relaxation characteristic of the ceramic, thereby obtaining higher dielectric and piezoelectric properties.
The second aspect of the present invention provides a method for preparing the PMNZT-based piezoelectric ceramic having a high piezoelectric coefficient according to the present invention, comprising the steps of:
1) According to MgNb 2 O 6 Stoichiometric ratio of (MgCO), will 3 ) 4 ·Mg(OH) 2 ·xH 2 O and Nb 2 O 5 Mixing, ball milling, drying and calcining to obtain a precursor MgNb 2 O 6 ；
2) According to the stoichiometric ratio of the chemical general formula, adding PbO and TiO 2 、ZrO 2 、Ln 2 O 3 And the precursor MgNb 2 O 6 Mixing and ball-milling to obtain slurry A;
3) Drying, grinding and presintering the slurry A to obtain presintering powder;
4) Mixing an organic binder and the pre-sintered powder, and performing ball milling to obtain slurry B;
5) Drying, grinding and sieving the slurry B, and then pressing and forming to obtain a ceramic green body;
6) Removing the organic binder from the ceramic green body by glue removal, and sintering at high temperature to obtain sintered ceramic;
7) And polishing the sintered ceramic, and then carrying out silver coating and high-voltage polarization on the surfaces of two sides of the polished sintered ceramic to obtain the PMNZT-based piezoelectric ceramic with the high piezoelectric coefficient.
Preferably, the calcining temperature in the step 1) is 1100-1200 ℃, and the calcining time is 2-6h.
Preferably, the ball milling medium adopted by the ball milling is absolute ethyl alcohol or water.
Preferably, the grinding balls adopted by the ball milling are zirconia grinding balls; the mass ratio of the materials to the grinding balls is 1 (10-12); the mass ratio of the materials to the ball milling medium is 1 (1-3); the ball milling time is 8-12h.
Preferably, the drying temperature is 100-150 ℃, and the drying time is 2-6h.
Preferably, the conditions of the pre-firing in the step 3) include: the presintering temperature is 800-850 ℃, and the presintering time is 1-2h.
Preferably, the organic binder in step 4) comprises PVA, PVB or Rhoplex solution; the addition amount of the organic binder is 1-5 wt% of the pre-sintering powder.
Preferably, the conditions for discharging the rubber in the step 6) comprise: the temperature is 550-650 ℃, the heat preservation time is 1-2h, and the heating rate is 1-2 ℃/min.
Preferably, the conditions of the high-temperature sintering in step 6) include: the temperature is 1200-1270 ℃, the heat preservation time is 1-2h, and the heating rate is 2-10 ℃/min.
Preferably, the high voltage polarization conditions in step 7) include: the polarization temperature is room temperature, the polarization electric field is 10-20kV/cm, and the polarization time is 5-10min.
A third aspect of the invention provides a piezoelectric device in which the PMNZT-based piezoelectric ceramic of high piezoelectric coefficient according to the invention is included; the piezoelectric device is a sensor, a driver, a transformer or a transducer.
Compared with the prior art, the invention has the following beneficial effects:
according to the PMNZT-based piezoelectric ceramic with the high piezoelectric coefficient, PMNZT ternary ceramic with excellent performance is selected as a substrate, trivalent ions with the radius slightly smaller than that of Pb ions are introduced into the A position, lattice distortion is caused, and the relaxation characteristics of the ceramic are enhanced, so that higher dielectric and piezoelectric properties are obtained; positive piezoelectric coefficient d of the piezoelectric ceramic 33 Up to 1040pC/N, inverse piezoelectric coefficient d 33 * Up to 1310pm/V, dielectric constant epsilon 33 4530-6460, dielectric loss tan delta less than 0.03, and planar electromechanical coupling coefficient k p Is more than 0.70, and the preparation process of the piezoelectric ceramic is simple, and has wide application prospect.
Drawings
FIG. 1 is an XRD pattern of a piezoelectric ceramic obtained in example 1 of the present invention;
FIG. 2 is a graph showing the tendency of the dielectric properties of the piezoelectric ceramic obtained in example 1 of the present invention to vary with temperature;
FIG. 3 is a field strain diagram of a piezoelectric ceramic obtained in example 1 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The raw materials, reagents and apparatuses used in the following examples are all available from conventional commercial sources or can be obtained by existing known methods, unless otherwise specified.
The room temperature in the present invention means 25. + -. 5 ℃.
Example 1
A PMNZT-based piezoelectric ceramic with high piezoelectric coefficient has a chemical formula: pb 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 。
Pb of the present example 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 The preparation method of the piezoelectric ceramic comprises the following steps:
1) According to MgNb 2 O 6 The stoichiometric ratio of (a) to (b), will (MgCO) 3 ) 4 ·Mg(OH) 2 ·xH 2 O and Nb 2 O 5 Mixing, ball milling in a ball milling tank, drying at 100 deg.c, calcining at 1100 deg.c for 6 hr to obtain precursor MgNb 2 O 6 (ii) a Wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 10h;
2) According to Pb 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 In a stoichiometric ratio of PbO, tiO 2 、ZrO 2 、Eu 2 O 3 And a precursor MgNb 2 O 6 Mixing, and then placing the mixture into a ball milling tank for ball milling to obtain slurry A; wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 10h;
3) Drying the slurry A at 100 ℃, then putting the slurry A into an agate mortar for grinding, and then putting the ground slurry A into an alumina crucible for presintering to obtain presintering powder; wherein the presintering temperature is 850 ℃, and the presintering time is 2 hours;
4) Mixing Rhoplex binder and the pre-sintered powder, and then putting the mixture into a ball milling tank for ball milling to obtain slurry B; wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 10h; the addition amount of the Rhoplex binder is 3wt% of the presintering powder;
5) Drying the slurry B at 100 ℃, then putting the dried slurry B into an agate mortar for grinding, and pressing and forming after sieving to obtain a ceramic green body;
6) Putting the ceramic green body into a muffle furnace, heating to 600 ℃ at the speed of 1 ℃/min, preserving heat for 2 hours, removing the Rhoplex binder, heating to 1250 ℃ at the speed of 2 ℃/min, preserving heat for 2 hours, and naturally cooling to obtain sintered ceramic;
7) Polishing the sintered ceramic to a thickness of 1.2mm, silver-coating the two side surfaces of the polished sintered ceramic, and performing high-pressure polarization to obtain Pb 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 Piezoelectric ceramics; wherein the polarization temperature is room temperature, the polarization electric field is 20kV/cm, and the polarization time is 5min.
And (3) testing and characterizing:
1. pb obtained in example 1 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 After the piezoelectric ceramic was pulverized, the material was subjected to X-ray diffraction (XRD), and the test results are shown in fig. 1. The ordinate "Intensity" of fig. 1 represents the diffraction Intensity; the abscissa "2 θ" represents the diffraction angle. It can be seen from figure 1 that the material is a single perovskite structure, with no pyrochlore or other heterophases being produced, and also showing that the dopant ions are able to enter into the lattice of the ceramic.
2. Pb obtained in example 1 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 Piezoelectric ceramics insert d 33 Measuring in a quasi-static analyzer to obtain a piezoelectric constant of 1040pC/N; dielectric constant ε at room temperature as measured by 4294A impedance analyzer 33 6460, dielectric loss tan delta of 0.021, planar electromechanical coupling coefficient k p Is 0.73. The dielectric temperature spectrum measured by the dielectric temperature measurement system is shown in FIG. 2. The left ordinate "Dielectric property" of fig. 2 represents the relative Dielectric constant; the right ordinate "Loss factor" represents dielectric Loss; the abscissa "Temperature" represents the test Temperature. It can be seen from fig. 2 that the dielectric constant shows a tendency of increasing and then decreasing with the increase of temperature, and shows a maximum value around 142 ℃, the dielectric constant is about 42000, and the dielectric constant also shows a stronger relaxation characteristic.
3. Pb obtained in example 1 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 Piezoelectric ceramicsThe porcelain was subjected to field strain property test, and the test results are shown in fig. 3. The inverse piezoelectric Strain coefficient of 1310pm/V can be calculated from the slope ratio Strain/Electric field, with the abscissa "Electric field" being the applied Electric field and the ordinate "Strain" being the Strain in FIG. 3.
Pb obtained in example 1 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 The performance of the piezoelectric ceramic was compared with that of the piezoelectric ceramic having better dielectric and piezoelectric properties (as comparative examples 1 to 5) obtained in the prior art of other companies and the ceramic material obtained in example 2 of the patent publication No. CN114436654A (as comparative example 6), and the results are shown in Table 1.
TABLE 1
The data in Table 1 show that the piezoelectric ceramic material obtained in example 1 of the present invention has a higher piezoelectric coefficient d than "soft" piezoelectric ceramic materials of other companies 33 And the material is a 'soft' piezoelectric ceramic material with excellent performance, wherein the '1040 pC/N' is defined by the formula I. Meanwhile, the inverse piezoelectric coefficient d is obtained in the piezoelectric strain test process 33 * =1310pm/V compared with the comparative example 6 doped with PbO, and the ceramic material prepared by adopting a complex tape casting texture preparation method has the inverse piezoelectric coefficient d obtained by the comparative example 6 33 * =1100pm/V, inventive example 1 employs Eu 2 O 3 The doping is more excellent in performance, simple in preparation process, low in cost and easy for mass production.
Example 2
A PMNZT-based piezoelectric ceramic with high piezoelectric coefficient has a chemical formula: pb 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.53 Zr 0.15 Ti 0.32 O 3 。
Pb of the present example 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.53 Zr 0.15 Ti 0.32 O 3 The preparation method of the piezoelectric ceramic comprises the following steps:
1) According to MgNb 2 O 6 The stoichiometric ratio of (a) to (b), will (MgCO) 3 ) 4 ·Mg(OH) 2 ·xH 2 O and Nb 2 O 5 Mixing, ball milling in a ball milling tank, drying at 100 deg.c, calcining at 1100 deg.c for 4 hr to obtain precursor MgNb 2 O 6 (ii) a Wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 10h;
2) According to Pb 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.53 Zr 0.15 Ti 0.32 O 3 In a stoichiometric ratio of PbO, tiO 2 、ZrO 2 、Eu 2 O 3 And a precursor MgNb 2 O 6 Mixing, and then placing the mixture into a ball milling tank for ball milling to obtain slurry A; wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 10h;
3) Drying the slurry A at 120 ℃, then putting the dried slurry A into an agate mortar for grinding, and then putting the ground slurry A into an alumina crucible for presintering to obtain presintering powder; wherein the presintering temperature is 850 ℃, and the presintering time is 2 hours;
4) Mixing Rhoplex binder and the pre-sintered powder, and then putting the mixture into a ball milling tank for ball milling to obtain slurry B; wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 10h; the addition amount of the Rhoplex binder is 2wt% of the pre-sintered powder;
5) Drying the slurry B at 120 ℃, then putting the dried slurry B into an agate mortar for grinding, sieving and then pressing for forming to obtain a ceramic green body;
6) Putting the ceramic green body into a muffle furnace, heating to 600 ℃ at the speed of 1 ℃/min, preserving heat for 2h, removing the Rhoplex binder, heating to 1250 ℃ at the speed of 2 ℃/min, preserving heat for 2h, and naturally cooling to obtain sintered ceramic;
7) Grinding and polishing the sintered ceramic to a thickness of 1.2mm, and then putting the two side surfaces of the polished sintered ceramic inSilver coating, high voltage polarization to obtain Pb 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.53 Zr 0.15 Ti 0.32 O 3 Piezoelectric ceramics; wherein the polarization temperature is room temperature, the polarization electric field is 20kV/cm, and the polarization time is 5min.
Pb obtained in example 2 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.53 Zr 0.15 Ti 0.32 O 3 Piezoelectric ceramics insert d 33 Measuring in a quasi-static analyzer to obtain a piezoelectric constant of 1010pC/N; dielectric constant ε at room temperature as measured by 4294A impedance analyzer 33 5330, dielectric loss tan delta of 0.027, planar electromechanical coupling coefficient k p Is 0.72.
Example 3
A PMNZT-based piezoelectric ceramic with high piezoelectric coefficient has a chemical formula as follows: pb 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.54 Zr 0.15 Ti 0.31 O 3 。
Pb of this example 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.54 Zr 0.15 Ti 0.31 O 3 The preparation method of the piezoelectric ceramic comprises the following steps:
1) According to MgNb 2 O 6 The stoichiometric ratio of (a) to (b), will (MgCO) 3 ) 4 ·Mg(OH) 2 ·xH 2 O and Nb 2 O 5 Mixing, ball milling in a ball milling tank, drying at 150 deg.c, calcining at 1100 deg.c for 6 hr to obtain precursor MgNb 2 O 6 (ii) a Wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the materials to the water is 1:1; the ball milling time is 12h;
2) According to Pb 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.54 Zr 0.15 Ti 0.31 O 3 Stoichiometric ratio of (B) to PbO, tiO 2 、ZrO 2 、Eu 2 O 3 And a precursor MgNb 2 O 6 Mixing, and then placing the mixture into a ball milling tank for ball milling to obtain slurry A; whereinThe mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the materials to the water is 1:1; the ball milling time is 12h;
3) Drying the slurry A at 150 ℃, then putting the slurry A into an agate mortar for grinding, and then putting the ground slurry A into an alumina crucible for presintering to obtain presintering powder; wherein the presintering temperature is 850 ℃, and the presintering time is 2 hours;
4) Mixing PVA binder and presintering powder, and then putting the mixture into a ball milling tank for ball milling to obtain slurry B; wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the materials to the water is 1:1; the ball milling time is 12h; the addition amount of the PVA binder is 1wt% of the pre-sintering powder;
5) Drying the slurry B at 150 ℃, then putting the dried slurry B into an agate mortar for grinding, and pressing and forming after sieving to obtain a ceramic green body;
6) Putting the ceramic green body into a muffle furnace, heating to 550 ℃ at the speed of 1 ℃/min, preserving heat for 2h, removing PVA binder, heating to 1270 ℃ at the speed of 10 ℃/min, preserving heat for 1h, and naturally cooling to obtain sintered ceramic;
7) Polishing the sintered ceramic to a thickness of 1.2mm, silver-coating the two side surfaces of the polished sintered ceramic, and performing high-pressure polarization to obtain Pb 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.54 Zr 0.15 Ti 0.31 O 3 Piezoelectric ceramics; wherein the polarization temperature is room temperature, the polarization electric field is 10kV/cm, and the polarization time is 10min.
Pb obtained in example 3 0.975 Eu 0.025 (Mg 1/3 Nb 2/3 ) 0.54 Zr 0.15 Ti 0.31 O 3 Piezoelectric ceramics insert d 33 Measuring in a quasi-static analyzer to obtain a piezoelectric constant of 950pC/N; dielectric constant ε at room temperature as measured by 4294A impedance analyzer 33 4530, dielectric loss tan delta of 0.024, planar electromechanical coupling coefficient k p Is 0.71.
Example 4
A PMNZT-based piezoelectric ceramic with high piezoelectric coefficient has a chemical formula as follows: pb 0.975 Nd 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 。
Pb of the present example 0.975 Nd 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 The preparation method of the piezoelectric ceramic comprises the following steps:
1) According to MgNb 2 O 6 Stoichiometric ratio of (MgCO), will 3 ) 4 ·Mg(OH) 2 ·xH 2 O and Nb 2 O 5 Mixing, ball milling in a ball milling tank, drying at 150 deg.c, calcining at 1200 deg.c for 2 hr to obtain precursor MgNb 2 O 6 (ii) a Wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the materials to the water is 1:1; the ball milling time is 10h;
2) According to Pb 0.975 Nd 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 Stoichiometric ratio of (B) to PbO, tiO 2 、ZrO 2 、Nd 2 O 3 And a precursor MgNb 2 O 6 Mixing, and then placing the mixture into a ball milling tank for ball milling to obtain slurry A; wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the materials to the water is 1:1; the ball milling time is 10h;
3) Drying the slurry A at 150 ℃, then putting the slurry A into an agate mortar for grinding, and then putting the ground slurry A into an alumina crucible for presintering to obtain presintering powder; wherein the presintering temperature is 850 ℃, and the presintering time is 1h;
4) Mixing PVB binder and pre-sintered powder, and then putting the mixture into a ball milling tank for ball milling to obtain slurry B; wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 10h; the addition amount of the PVB binder is 4wt% of the pre-sintered powder;
5) Drying the slurry B at 150 ℃, then putting the dried slurry B into an agate mortar for grinding, and pressing and forming after sieving to obtain a ceramic green body;
6) Putting the ceramic green body into a muffle furnace, heating to 650 ℃ at the speed of 2 ℃/min, preserving heat for 1h, removing PVB binder, heating to 1200 ℃ at the speed of 2 ℃/min, preserving heat for 2h, and naturally cooling to obtain sintered ceramic;
7) Polishing the sintered ceramic to a thickness of 1.2mm, silver-coating the two side surfaces of the polished sintered ceramic, and performing high-pressure polarization to obtain Pb 0.975 Nd 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 Piezoelectric ceramics; wherein the polarization temperature is room temperature, the polarization electric field is 15kV/cm, and the polarization time is 8min.
Pb obtained in example 4 0.975 Nd 0.025 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 Piezoelectric ceramics insert d 33 Measuring in a quasi-static analyzer to obtain a piezoelectric constant 990pC/N; dielectric constant ε at room temperature as measured by 4294A impedance analyzer 33 5840, dielectric loss tan delta of 0.023, planar electromechanical coupling coefficient k p Is 0.72.
Example 5
A PMNZT-based piezoelectric ceramic with high piezoelectric coefficient has a chemical formula: pb 0.975 Nd 0.0125 Eu 0.0125 (Mg 1/ 3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 。
Pb of this example 0.975 Nd 0.0125 Eu 0.0125 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 The preparation method of the piezoelectric ceramic comprises the following steps:
1) According to MgNb 2 O 6 The stoichiometric ratio of (a) to (b), will (MgCO) 3 ) 4 ·Mg(OH) 2 ·xH 2 O and Nb 2 O 5 Mixing, ball milling in a ball milling tank, drying at 100 deg.c, calcining at 1100 deg.c for 6 hr to obtain precursor MgNb 2 O 6 (ii) a Wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 8h;
2) According to Pb 0.975 Nd 0.0125 Eu 0.0125 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 In a stoichiometric ratio of PbO, tiO 2 、ZrO 2 、Nd 2 O 3 、Eu 2 O 3 And a precursor MgNb 2 O 6 Mixing, and then placing the mixture into a ball milling tank for ball milling to obtain slurry A; wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 8h;
3) Drying the slurry A at 120 ℃, then putting the dried slurry A into an agate mortar for grinding, and then putting the ground slurry A into an alumina crucible for presintering to obtain presintering powder; wherein the presintering temperature is 850 ℃, and the presintering time is 2 hours;
4) Mixing Rhoplex binder and the pre-sintered powder, and then putting the mixture into a ball milling tank for ball milling to obtain slurry B; wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 8h; the addition amount of the Rhoplex binder is 2wt% of the presintering powder;
5) Drying the slurry B at 100 ℃, then putting the dried slurry B into an agate mortar for grinding, and pressing and forming after sieving to obtain a ceramic green body;
6) Putting the ceramic green body into a muffle furnace, heating to 600 ℃ at the speed of 1 ℃/min, preserving heat for 2 hours, removing the Rhoplex binder, heating to 1250 ℃ at the speed of 2 ℃/min, preserving heat for 2 hours, and naturally cooling to obtain sintered ceramic;
7) Polishing the sintered ceramic to a thickness of 1.2mm, silver-coating the two side surfaces of the polished sintered ceramic, and performing high-pressure polarization to obtain Pb 0.975 Nd 0.0125 Eu 0.0125 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 Piezoelectric ceramics; wherein the polarization temperature is room temperature, the polarization electric field is 20kV/cm, and the polarization time is 5min.
Pb obtained in example 5 0.975 Nd 0.0125 Eu 0.0125 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 Piezoelectric ceramics insert d 33 Measuring in a quasi-static analyzer to obtain a piezoelectric constant of 1010pC/N;dielectric constant ε at room temperature as measured by 4294A impedance analyzer 33 6220, dielectric loss tan delta of 0.022, and planar electromechanical coupling coefficient k p Is 0.72.
Comparative example 7 (different from example 1 in that y is not within the range defined by the present invention, y = 0.03)
A PMNZT-based piezoelectric ceramic with high piezoelectric coefficient has a chemical formula: pb 0.97 Eu 0.03 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 。
Pb of this comparative example 0.97 Eu 0.03 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 The preparation method of the piezoelectric ceramic comprises the following steps:
1) According to MgNb 2 O 6 Stoichiometric ratio of (MgCO), will 3 ) 4 ·Mg(OH) 2 ·xH 2 O and Nb 2 O 5 Mixing, ball milling in a ball milling tank, drying at 100 deg.c, calcining at 1100 deg.c for 6 hr to obtain precursor MgNb 2 O 6 (ii) a Wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 10h;
2) According to Pb 0.97 Eu 0.03 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 In a stoichiometric ratio of PbO, tiO 2 、ZrO 2 、Eu 2 O 3 And a precursor MgNb 2 O 6 Mixing, and then placing the mixture into a ball milling tank for ball milling to obtain slurry A; wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 10h;
3) Drying the slurry A at 100 ℃, then putting the slurry A into an agate mortar for grinding, and then putting the ground slurry A into an alumina crucible for presintering to obtain presintering powder; wherein the presintering temperature is 850 ℃, and the presintering time is 2 hours;
4) Mixing Rhoplex binder and the pre-sintered powder, and then putting the mixture into a ball milling tank for ball milling to obtain slurry B; wherein the mass ratio of the material to the zirconia grinding ball is 1; the mass ratio of the material to the absolute ethyl alcohol is 1:1; the ball milling time is 10h; the addition amount of the Rhoplex binder is 3wt% of the presintering powder;
5) Drying the slurry B at 100 ℃, then putting the dried slurry B into an agate mortar for grinding, and pressing and forming after sieving to obtain a ceramic green body;
6) Putting the ceramic green body into a muffle furnace, heating to 600 ℃ at the speed of 1 ℃/min, preserving heat for 2 hours, removing the Rhoplex binder, heating to 1250 ℃ at the speed of 2 ℃/min, preserving heat for 2 hours, and naturally cooling to obtain sintered ceramic;
7) Polishing the sintered ceramic to a thickness of 1.2mm, silver-coating the two side surfaces of the polished sintered ceramic, and performing high-pressure polarization to obtain Pb 0.97 Eu 0.03 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 Piezoelectric ceramics; wherein the polarization temperature is room temperature, the polarization electric field is 20kV/cm, and the polarization time is 5min.
Pb obtained in comparative example 7 0.97 Eu 0.03 (Mg 1/3 Nb 2/3 ) 0.52 Zr 0.15 Ti 0.33 O 3 Piezoelectric ceramics insert d 33 Measuring in a quasi-static analyzer to obtain a piezoelectric constant of 760pC/N; dielectric constant ε at room temperature as measured by 4294A impedance analyzer 33 4960, dielectric loss tan delta of 0.24, planar electromechanical coupling coefficient k p Is 0.65.
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that the present invention is not limited to the details of the embodiments shown and described, but is capable of numerous modifications and substitutions without departing from the spirit of the present invention and within the scope of the appended claims.
Claims (10)
1. The PMNZT-based piezoelectric ceramic with high piezoelectric coefficient is characterized in that the chemical general formula of the PMNZT-based piezoelectric ceramic with high piezoelectric coefficient is as follows: pb (1-y) Ln y (Mg 1/3 Nb 2/3 ) (0.85-x) Zr 0.15 Ti x O 3 Wherein x is more than or equal to 0.31 and less than or equal to 0.34,0.02 and less than or equal to 0.025, x and y both represent mole fractions, and Ln is one or two of Nd and Eu elements.
2. The method for preparing a PMNZT-based piezoelectric ceramic having a high piezoelectric coefficient according to claim 1, comprising the steps of:
1) According to MgNb 2 O 6 The stoichiometric ratio of (a) to (b), will (MgCO) 3 ) 4 ·Mg(OH) 2 ·xH 2 O and Nb 2 O 5 Mixing, ball-milling, drying and calcining to obtain a precursor MgNb 2 O 6 ；
2) According to the stoichiometric ratio of the chemical general formula, pbO and TiO are mixed 2 、ZrO 2 、Ln 2 O 3 And the precursor MgNb 2 O 6 Mixing and ball-milling to obtain slurry A;
3) Drying, grinding and presintering the slurry A to obtain presintering powder;
4) Mixing an organic binder and the pre-sintered powder, and performing ball milling to obtain slurry B;
5) Drying, grinding and screening the slurry B, and then pressing and forming to obtain a ceramic green body;
6) Removing the organic binder from the ceramic green body by glue removal, and sintering at high temperature to obtain sintered ceramic;
7) And polishing the sintered ceramic, and then carrying out silver coating and high-voltage polarization on the surfaces of two sides of the polished sintered ceramic to obtain the PMNZT-based piezoelectric ceramic with the high piezoelectric coefficient.
3. The preparation method of claim 2, wherein the calcining temperature in the step 1) is 1100-1200 ℃, and the calcining time is 2-6h.
4. The preparation method according to claim 2, wherein the ball milling medium adopted in the ball milling process is absolute ethyl alcohol or water.
5. The method of claim 2, wherein the pre-firing conditions in step 3) include: the presintering temperature is 800-850 ℃, and the presintering time is 1-2h.
6. The method of claim 2, wherein the organic binder in step 4) comprises a PVA, PVB, or Rhoplex solution; the addition amount of the organic binder is 1-5 wt% of the pre-sintering powder.
7. The method according to claim 2, wherein the conditions for the stripping in step 6) include: the temperature is 550-650 ℃, the heat preservation time is 1-2h, and the heating rate is 1-2 ℃/min.
8. The method according to claim 2, wherein the conditions of the high-temperature sintering in step 6) include: the temperature is 1200-1270 ℃, the heat preservation time is 1-2h, and the heating rate is 2-10 ℃/min.
9. The method of claim 2, wherein the high voltage polarization conditions in step 7) include: the polarization temperature is room temperature, the polarization electric field is 10-20kV/cm, and the polarization time is 5-10min.
10. A piezoelectric device comprising the high piezoelectric coefficient PMNZT-based piezoelectric ceramic of claim 1; the piezoelectric device is a sensor, a driver, a transformer or a transducer.
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