CN113773078A - High-power piezoelectric ceramic material and preparation method thereof - Google Patents
High-power piezoelectric ceramic material and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000919 ceramic Substances 0.000 claims abstract description 63
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- 239000000463 material Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 230000010287 polarization Effects 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 238000000465 moulding Methods 0.000 claims abstract description 10
- 238000007599 discharging Methods 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000002002 slurry Substances 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 12
- 235000015895 biscuits Nutrition 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000005684 electric field Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
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- 238000010168 coupling process Methods 0.000 claims description 4
- 238000005859 coupling reaction Methods 0.000 claims description 4
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 238000000875 high-speed ball milling Methods 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 10
- 229910052451 lead zirconate titanate Inorganic materials 0.000 abstract description 8
- 229910004481 Ta2O3 Inorganic materials 0.000 abstract description 5
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 abstract description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract description 5
- 229910052681 coesite Inorganic materials 0.000 abstract description 5
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 5
- 239000000377 silicon dioxide Substances 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052682 stishovite Inorganic materials 0.000 abstract description 5
- 229910052905 tridymite Inorganic materials 0.000 abstract description 5
- 239000012814 acoustic material Substances 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 3
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 abstract description 3
- 239000006104 solid solution Substances 0.000 abstract description 3
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Abstract
The invention relates to a high-power piezoelectric ceramic material and a preparation method thereof, wherein the main component of the piezoelectric ceramic material is lead zirconate titanate solid solution which can be undoped or doped and is selected from Fe2O3、Ta2O3、CaCO3、BaCO3And SiO2At least 2 and several additives. The method comprises the following steps: preparing materials: the ceramic formula is PbxSr1‑x(ZryTi1‑y)O3+aFe2O3+bTa2O3+cCaCO3+dBaCO3+eSiO2Mixing, pre-burningSecondary ball milling, plasticizing, molding and plastic discharging, sintering, electrode loading and polarization treatment and piezoelectric performance measurement. The piezoelectric ceramic material of the invention introduces Fe on the basis of PZT series piezoelectric ceramics2O3、Ta2O3、CaCO3、BaCO3And SiO2The substances are beneficial to improving various piezoelectric properties of the ceramic, and the ceramic material obtained by the preparation method disclosed by the invention has low loss and high dielectricity, and is suitable for high-power underwater acoustic materials.
Description
Technical Field
The invention relates to a piezoelectric ceramic material technology, in particular to a high-power piezoelectric ceramic material and a preparation method thereof.
Background
PZT piezoelectric ceramic material is a functional material with wide application, and can realize the mutual conversion of electric energy and mechanical energy through piezoelectric effect. PZT-based piezoelectric ceramics have the advantages of high electromechanical coupling coefficient, easy processing into complex shapes, low price, easy mass production, etc., and have been widely used in electronic devices. However, the existing piezoelectric ceramic material can not meet the comprehensive requirements of practical application on material performance. With the rapid development of modern industry, higher requirements are put on high-performance and low-loss piezoelectric ceramics.
At present, in order to improve the working performance of piezoelectric ceramics, PZT series piezoelectric ceramics are doped and modified according to different influences of different doped ions on the structure and the performance of materials. Since the mechanism of action of doping is very complex, the search for the intrinsic rule between microstructure and electrical properties has been the focus of research by researchers in recent years.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the problem that the existing piezoelectric ceramic material cannot meet the comprehensive requirements of practical application on material performance, thereby providing a high-power piezoelectric ceramic material and a preparation method thereof.
In order to solve the technical problems, the invention provides a high-power piezoelectric ceramic material and a preparation method thereof, wherein the main component of the high-power piezoelectric ceramic material is lead zirconate titanate solid solution which can be undoped or doped with Fe2O3、Ta2O3、CaCO3、BaCO3And SiO2At least 2 and several additives. The method comprises the following steps:
step S1, batching: the ceramic formula is PbxSr1-x(ZryTi1-y)O3+aFe2O3+bTa2O3+cCaCO3+dBaCO3+eSiO2(ii) a Wherein x and y are molar ratios, a, b, c, d and e are weight ratios, x is more than or equal to 0.91 and less than or equal to 0.97, y is more than or equal to 0.51 and less than or equal to 0.55, a is more than or equal to 0.15 and less than or equal to 0.25, b is more than or equal to 0.2 and less than or equal to 0.3, c is more than or equal to 0.5 and less than or equal to 0.45, d is more than or equal to 0.15 and less than or equal to 0.2, and e is more than or equal to 0.1 and less than or equal to 0.15, and the proportions of the components are calculated according to the chemical molecular formula and prepared;
step S2, mixing: ball-milling and mixing materials by adopting a traditional wet method, and adding ceramic powder and deionized water into a stirring barrel according to the mass ratio of 100: 45;
step S3, burn-in: the process of forming piezoelectric ceramics is a typical chemical reaction process, and at a temperature lower than the melting point, Pb atoms can be diffused into crystals of other materials to form PbZrTiO3；
Step S4, secondary ball milling: weighing the ceramic powder after the pre-sintering treatment, pouring the ceramic powder into deionized water, and uniformly stirring to prepare mixed ceramic slurry;
step S5, plasticizing: taking the thinned ceramic slurry out of the charging barrel; ball-milling and stirring the ceramic slurry and PVA solution which accounts for about 5 percent of the weight of the material, uniformly mixing, introducing the ceramic slurry into a spray granulator, and further sieving the prepared powder by using a 100-mesh screen;
step S6, molding and plastic discharge: pre-pressing and molding the powder, and plastic discharging: putting the ceramic biscuit into a muffle furnace, setting the highest temperature to be 750 ℃, and further removing a forming agent in the ceramic biscuit;
step S7, sintering: setting the sintering temperature to 1290-;
step S8, upper electrode and polarization processing, upper electrode: carrying out silver impregnation treatment on the surface of the piezoelectric ceramic to form a metal film, and carrying out polarization treatment: applying a strong direct current electric field to the piezoelectric ceramic;
step S9, piezoelectric property measurement: e.g. d33Dielectric loss tan delta and electromechanical coupling coefficient Kp。
In an embodiment of the invention, slurry is adopted in the material mixing step and is stirred in a stirring barrel for 5min in advance, high-speed ball milling is started without exception after low-speed ball milling is carried out for 30s, the ball milling time is set to be 4h, and the slurry is dried for later use after the ball milling is finished.
In one embodiment of the invention, the mixed ceramic slurry is filled into a cylinder of a ball mill for secondary refining treatment for 24 hours in the secondary ball milling step.
In the molding and plastic discharging steps, the wafer is pre-pressed to form the wafer with the size of 20x1 mm.
In an embodiment of the present invention, after the piezoelectric ceramic is subjected to the polarization treatment step, ferroelectric domains inside the material of the piezoelectric ceramic are turned, all the ferroelectric domains in the piezoelectric ceramic are arranged in the direction of an electric field, and only the piezoelectric ceramic subjected to the polarization treatment has a piezoelectric effect.
Compared with the prior art, the technical scheme of the invention has the following advantages: the piezoelectric ceramic material of the invention introduces Fe on the basis of PZT series piezoelectric ceramics2O3、Ta2O3、CaCO3、BaCO3And SiO2The substances are beneficial to improving various piezoelectric properties of the ceramic, and the ceramic material obtained by the preparation method disclosed by the invention has low loss and high dielectricity, and is suitable for high-power underwater acoustic materials.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference will now be made in detail to the present disclosure, examples of which are illustrated in the accompanying drawings.
FIG. 1 is a flow chart of a high-power piezoelectric ceramic material and a preparation method thereof.
Detailed Description
As shown in FIG. 1, the present embodiment provides a high-power piezoelectric ceramic material and a method for preparing the same, wherein the main component is lead zirconate titanate solid solution, which may be undoped or doped with Fe2O3、Ta2O3、CaCO3、BaCO3And SiO2At least 2 and several additives. The method comprises the following steps:
step S1, batching: the ceramic formula is PbxSr1-x(ZryTi1-y)O3+aFe2O3+bTa2O3+cCaCO3+dBaCO3+eSiO2(ii) a Wherein x and y are molar ratios, a, b, c, d and e are weight ratios, x is more than or equal to 0.91 and less than or equal to 0.97, y is more than or equal to 0.51 and less than or equal to 0.55, a is more than or equal to 0.15 and less than or equal to 0.25, b is more than or equal to 0.2 and less than or equal to 0.3, c is more than or equal to 0.5 and less than or equal to 0.45, d is more than or equal to 0.15 and less than or equal to 0.2, and e is more than or equal to 0.1 and less than or equal to 0.15, and the proportions of the components are calculated according to the chemical molecular formula and prepared;
step S2, mixing: ball-milling and mixing materials by adopting a traditional wet method, and adding ceramic powder and deionized water into a stirring barrel according to the mass ratio of 100: 45;
step S3, burn-in: the process of forming piezoelectric ceramics is a typical chemical reaction process, and at a temperature lower than the melting point, Pb atoms can be diffused into crystals of other materials to form PbZrTiO3；
Step S4, secondary ball milling: weighing the ceramic powder after the pre-sintering treatment, pouring the ceramic powder into deionized water, and uniformly stirring to prepare mixed ceramic slurry;
step S5, plasticizing: taking the thinned ceramic slurry out of the charging barrel; ball-milling and stirring the ceramic slurry and PVA solution which accounts for about 5 percent of the weight of the material, uniformly mixing, introducing the ceramic slurry into a spray granulator, and further sieving the prepared powder by using a 100-mesh screen;
step S6, molding and plastic discharge: pre-pressing and molding the powder, and plastic discharging: placing the ceramic biscuit into a muffle furnace, setting the maximum temperature to be 750 ℃, further removing a forming agent in the ceramic biscuit, ensuring the sintering quality and improving the sintering density;
step S7, sintering: setting the sintering temperature to 1300 ℃ in the experiment, preserving the heat for 2 hours, and cooling along with the furnace;
step S8, upper electrode and polarization processing, upper electrode: carrying out silver impregnation treatment on the surface of the piezoelectric ceramic to form a metal film, and carrying out polarization treatment: applying a strong direct current electric field to the piezoelectric ceramic;
step S9, piezoelectric property measurement: e.g. d33Dielectric loss tan delta and electromechanical coupling coefficient Kp。
Wherein the experimental measurement results of the 20x1mm round wafer are as follows:
general performance parameters of the high-power piezoelectric material (P-8) of the underwater acoustic material are as follows:
and (4) conclusion:
the dielectric loss of the high-power ceramic material prepared by the method is tan delta (%) (0.25), and d is at normal temperature33The value is 285pC/N, k at room temperaturep59 percent, reaches the performance standard of the underwater acoustic material application. In addition, compared with the common high-power piezoelectric material, the material prepared by the method has higher dielectric constant and more application occasions.
And in the material mixing step, slurry is required to be stirred in a stirring barrel for 5min in advance, high-speed ball milling is started without abnormal operation after low-speed ball milling is carried out for 30s, the ball milling time is set to be 4h, and the slurry is dried for later use after the ball milling is finished.
And in the secondary ball milling step, the mixed ceramic slurry is filled into a charging barrel of the ball mill for secondary refining treatment for 24 hours.
In the molding and plastic discharging steps, the wafer is pre-pressed to form the wafer with the size of 20x1 mm.
After the piezoelectric ceramic is subjected to the polarization treatment step, ferroelectric domains in the piezoelectric ceramic are turned, all the ferroelectric domains in the piezoelectric ceramic are arranged in the direction of an electric field, and only the piezoelectric ceramic subjected to the polarization treatment has the piezoelectric effect.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (5)
1. A high-power piezoelectric ceramic material and a preparation method thereof are characterized by comprising the following steps:
step S1, batching: the ceramic formula is PbxSr1-x(ZryTi1-y)O3+aFe2O3+bTa2O3+cCaCO3+dBaCO3+eSiO2(ii) a Wherein x and y are molar ratios, a, b, c, d and e are weight ratios, x is more than or equal to 0.91 and less than or equal to 0.97, y is more than or equal to 0.51 and less than or equal to 0.55, a is more than or equal to 0.15 and less than or equal to 0.25, b is more than or equal to 0.2 and less than or equal to 0.3, c is more than or equal to 0.5 and less than or equal to 0.45, d is more than or equal to 0.15 and less than or equal to 0.2, and e is more than or equal to 0.1 and less than or equal to 0.15, and the proportions of the components are calculated according to the chemical molecular formula and prepared;
step S2, mixing: ball-milling and mixing materials by adopting a traditional wet method, and adding ceramic powder and deionized water into a stirring barrel according to the mass ratio of 100: 45;
step S3, burn-in: the process of forming piezoelectric ceramics is a typical chemical reaction process, and at a temperature lower than the melting point, Pb atoms can be diffused into crystals of other materials to form PbZrTiO3；
Step S4, secondary ball milling: weighing the ceramic powder after the pre-sintering treatment, pouring the ceramic powder into deionized water, and uniformly stirring to prepare mixed ceramic slurry;
step S5, plasticizing: taking the thinned ceramic slurry out of the charging barrel; ball-milling and stirring the ceramic slurry and PVA solution which accounts for about 5 percent of the weight of the material, uniformly mixing, introducing the ceramic slurry into a spray granulator, and further sieving the prepared powder by using a 100-mesh screen;
step S6, molding and plastic discharge: pre-pressing and molding the powder, and plastic discharging: putting the ceramic biscuit into a muffle furnace, setting the highest temperature to be 750 ℃, and further removing a forming agent in the ceramic biscuit;
step S7, sintering: setting the sintering temperature to 1290-;
step S8, upper electrode and polarization processing, upper electrode: carrying out silver impregnation treatment on the surface of the piezoelectric ceramic to form a metal film, and carrying out polarization treatment: applying a strong direct current electric field to the piezoelectric ceramic;
step S9, piezoelectric performanceMeasurement: e.g. d33Dielectric loss tan delta and electromechanical coupling coefficient Kp。
2. The high-power piezoelectric ceramic material and the preparation method thereof according to claim 1, wherein: and in the material mixing step, slurry is required to be stirred in a stirring barrel for 5min in advance, high-speed ball milling is started without abnormal operation after low-speed ball milling is carried out for 30s, the ball milling time is set to be 4h, and the slurry is dried for later use after the ball milling is finished.
3. The high-power piezoelectric ceramic material and the preparation method thereof according to claim 1, wherein: and in the secondary ball milling step, the mixed ceramic slurry is filled into a charging barrel of the ball mill for secondary refining treatment for 24 hours.
4. The high-power piezoelectric ceramic material and the preparation method thereof according to claim 1, wherein: in the molding and plastic discharging steps, the wafer is pre-pressed to form the wafer with the size of 20x1 mm.
5. The high-power piezoelectric ceramic material and the preparation method thereof according to claim 1, wherein: after the piezoelectric ceramic is subjected to the polarization treatment step, ferroelectric domains in the piezoelectric ceramic are turned, all the ferroelectric domains in the piezoelectric ceramic are arranged in the direction of an electric field, and only the piezoelectric ceramic subjected to the polarization treatment has the piezoelectric effect.
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