CN109503157B - Piezoelectric ceramic with high density and high piezoelectric constant - Google Patents
Piezoelectric ceramic with high density and high piezoelectric constant Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 60
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 229910019653 Mg1/3Nb2/3 Inorganic materials 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 12
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 230000008878 coupling Effects 0.000 claims description 9
- 238000010168 coupling process Methods 0.000 claims description 9
- 238000005859 coupling reaction Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 7
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 6
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 238000009694 cold isostatic pressing Methods 0.000 abstract description 6
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 8
- 239000002994 raw material Substances 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 4
- 229910000018 strontium carbonate Inorganic materials 0.000 description 4
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910020684 PbZr Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The invention discloses a high-density high-piezoelectric constant piezoelectric ceramic with a chemical formula of Pb1‑xMx(ZryTi1‑y)0.75(Ni1/ 3Nb2/3)0.2(Sb1/3Nb2/3)0.015(Mg1/3Nb2/3)0.035O3+zwt%Bi2O3Wherein x is the sum of the elements in M, x = 0.07-0.15, y = 0.45-0.55, z = 0.2-1, and M is Ba2+、Sr2+、Ca2+、La3+One or a combination of several of them. The piezoelectric ceramic is formed by dry bag type cold isostatic pressing, and the density of a ceramic green body can reach 5.4g/cm3The density uniformity is good, the consistency of the ceramic performance is high, and the density of the sintered ceramic can reach 98 percent of the theoretical density. The invention overcomes the problems of low density and non-uniformity of the common piezoelectric ceramics after sintering, improves the piezoelectric constant of the piezoelectric ceramics and the consistency thereof, and obtains the piezoelectric ceramics with the piezoelectric constant of 1053 pC/N; the piezoelectric ceramic has high piezoelectric constant and good consistency, and can be widely applied to the field of high-tech piezoelectric products with high content of high-tech, such as piezoelectric sensors, piezoelectric actuators and the like.
Description
Technical Field
The invention belongs to the field of high-voltage-constant piezoelectric ceramics of material science, and particularly relates to a compact high-voltage-constant piezoelectric ceramic and a preparation method thereof.
Background
The piezoelectric ceramic is widely applied to various fields of material engineering, acoustoelectric and human daily life and production, and the most applied at present is perovskite type zirconium titaniumAcid lead (PbZr)xTi1-xO3Abbreviated as PZT) or a multi-element piezoelectric ceramic formed by doping other components on the basis of PZT, but the piezoelectric constant of the piezoelectric ceramic is generally 300 pC/N-800 pC/N, the electromechanical coupling coefficient is about 0.72, and the application in the field of high-sensitivity piezoelectric ceramic sensors and piezoelectric ceramic actuators needing high deflection is limited. Therefore, the research on the high-quality piezoelectric ceramics with larger piezoelectric constants can improve the performance indexes of piezoelectric devices such as piezoelectric sensors and piezoelectric actuators and lay a better foundation for the design of the devices.
At present, researchers have carried out the formulation research of ternary, quaternary and quinary of PZT ceramics, but the overall performance is still low, such as PZT-PNN series piezoelectric ceramics researched by Pengzhite and the like, the piezoelectric constant is 680 pC/N; the piezoelectric constant of PMN-PNN-PT series piezoelectric ceramics researched by Yu Chen et al reaches 780 pC/N; H. the PNN-PHT series piezoelectric ceramics researched by Tang et al have piezoelectric constants reaching 970pC/N, but have planar electromechanical coupling coefficients of only 0.65. Meanwhile, the density and uniformity of the piezoelectric ceramic affect the uniformity of the piezoelectric constant of the piezoelectric ceramic and the planar electromechanical coupling coefficient.
Therefore, when the PZT piezoelectric ceramic is researched, five-element components comprising PNN, PSN, PMN and PZT are adopted to find the MPB region of the material to obtain the optimal electrical performance, and the sintering density value and uniformity of the material are improved through dry bag type cold isostatic pressing to obtain the piezoelectric ceramic with high density and high voltage constant.
Disclosure of Invention
Aiming at the problems of low density, low piezoelectric constant and poor uniformity of the existing piezoelectric ceramic material. The invention provides a high-performance piezoelectric ceramic material with high density, high piezoelectric constant, high electromechanical coupling coefficient and high uniformity and a preparation method thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a high-density high-piezoelectric constant piezoelectric ceramic has the chemical formula: pb1-xMx(ZryTi1-y)0.75(Ni1/ 3Nb2/3)0.2(Sb1/3Nb2/3)0.015(Mg1/3Nb2/3)0.035O3+zwt%Bi2O3Wherein x is the sum of the elements in M, x = 0.07-0.15, y = 0.45-0.55, z = 0.2-1, and M is Ba2+、Sr2+、Ca2+、La3+One or a combination of more of the above; the preparation method of the high-density high-voltage constant piezoelectric ceramic comprises the following steps:
(1) adding Pb3O4、ZrO2、TiO2、NiO、Sb2O3、Nb2O5MgO, M and Bi2O3Weighing the materials according to a stoichiometric ratio;
(2) ball-milling, presintering, secondary ball-milling and drying the prepared powder material in the step (1) to prepare the required piezoelectric ceramic powder;
(3) adding a certain amount of deionized water and polyvinyl alcohol into the ceramic powder prepared in the step (2) for spray granulation;
(4) putting the ceramic powder prepared in the step (3) into a dry bag type cold isostatic press for pressing and molding to prepare the ceramic powder with the sintering density of more than or equal to 5.2g/cm3And testing the green density of the piezoelectric ceramic green body;
(5) keeping the green body at 550 ℃ for 4-6 hours to remove the glue, then heating to 1250-1300 ℃ at the speed of 3-5 ℃/min in the air atmosphere, and keeping the temperature for 2-4 hours to obtain the general formula Pb1-xMx(ZryTi1-y)0.75(Ni1/3Nb2/3)0.2(Sb1/ 3Nb2/3)0.015(Mg1/3Nb2/3)0.035O3+zwt%Bi2O3The piezoelectric ceramic of (1);
(6) the prepared piezoelectric ceramic is printed with silver and is polarized, and then the physical and electrical properties of the piezoelectric ceramic are tested.
Wherein the pressure in the step (4) is 60 MPa-120 MPa, and the green body forming density is 5.2g/cm3~5.5g/cm3Density uniformity of + -0.05 g/cm3(ii) a The sintered piezoelectric ceramic obtained in the step (5) is denseThe degree is more than 98% of the theoretical density; the piezoelectric constant of the piezoelectric ceramic prepared by the method reaches 950 pC/N-1053 pC/N, and the electromechanical coupling coefficient is not less than 0.75.
Drawings
FIG. 1: the density rho test chart of different batches of piezoelectric ceramics is provided in the embodiment 1 of the invention;
FIG. 2: example 1 piezoelectric constant d of piezoelectric ceramics of different batches33Measuring a view;
FIG. 3: the invention embodiment 1 is a relative density view of different batches of piezoelectric ceramics;
FIG. 4: embodiment 1 of the invention piezoelectric ceramics different batches of planar electromechanical coupling coefficient kpAnd (6) view measurement.
Detailed Description
The present invention is further described below in conjunction with the following embodiments and the accompanying drawings, it being understood that the drawings and the following embodiments are illustrative of the invention only and are not limiting.
Example 1:
with Pb3O4，SrCO3，BaCO3，ZrO2，TiO2，NiO，Nb2O5，Sb2O3，MgO，Bi2O3(analytically pure) as raw material according to Pb0.93Sr0.05Ba0.02(Zr0.5Ti0.5)0.75(Ni1/3Nb2/3)0.2(Sb1/3Nb2/3)0.015(Mg1/3Nb2/3)0.035O3+0.2wt%Bi2O3Weighing the raw materials according to the stoichiometric ratio, and testing the density of the green body after ball milling, pre-sintering, secondary ball milling and dry bag type cold isostatic pressing, wherein the specific density parameter of the green body is shown in figure 1; sintering at 1270 deg.C for 2h, polarizing, and testing physical and electrical properties, wherein the piezoelectric constant, relative density, and electromechanical coupling coefficient are shown in FIG. 2, FIG. 3, and FIG. 4, and other electrical properties are shown in Table 1.
Example 2:
with Pb3O4，SrCO3，BaCO3，ZrO2，TiO2，NiO，Nb2O5，Sb2O3，MgO，Bi2O3(analytically pure) as raw material according to Pb0.92Sr0.06Ba0.02(Zr0.5Ti0.5)0.75(Ni1/3Nb2/3)0.2(Sb1/3Nb2/3)0.015(Mg1/3Nb2/3)0.035O3+0.2wt%Bi2O3The chemical ratio of (A) is weighed, ball-milled, pre-sintered, secondary ball-milled, and dry-bag type cold isostatic pressing is carried out, then sintering is carried out for 2 hours at 1300 ℃, and after polarization, the physical properties and the electrical properties of the material are tested, and the results are shown in table 1.
Example 3:
with Pb3O4，SrCO3，BaCO3，ZrO2，TiO2，NiO，Nb2O5，Sb2O3，MgO，Bi2O3(analytically pure) as raw material according to Pb0.93Sr0.05Ba0.02(Zr0.48Ti0.52)0.75(Ni1/3Nb2/3)0.2(Sb1/3Nb2/3)0.015(Mg1/3Nb2/3)0.035O3+0.2wt%Bi2O3The chemical ratio of (A) is weighed, ball-milled, pre-sintered, secondary ball-milled, and dry-bag type cold isostatic pressing is carried out, then sintering is carried out for 2 hours at 1300 ℃, and after polarization, the physical properties and the electrical properties of the material are tested, and the results are shown in table 1.
Example 4:
with Pb3O4，SrCO3，BaCO3，ZrO2，TiO2，NiO，Nb2O5，Sb2O3，MgO，Bi2O3(analytically pure) as raw material according to Pb0.91Sr0.06Ba0.03(Zr0.48Ti0.52)0.75(Ni1/3Nb2/3)0.2(Sb1/3Nb2/3)0.015(Mg1/3Nb2/3)0.035O3+0.2wt%Bi2O3Stoichiometric ratio of (2) ballAfter grinding, pre-sintering, secondary ball milling and dry bag type cold isostatic pressing, sintering is carried out for 2 hours at 1300 ℃, and after polarization, the physical properties and the electrical properties are tested, and the results are shown in table 1.
Table 1: comparison of Performance parameters of bismuth layered high temperature leadless piezoelectric ceramics of different embodiments
| Examples | d33(pC/N） | εr | tanδ(%) | kp(%) | Relative density (%) |
| 1 | 1053 | 8000 | 3.9 | 0.78 | 98.7 |
| 2 | 1037 | 7000 | 4.7 | 0.79 | 98.5 |
| 3 | 1012 | 7500 | 3.7 | 0.77 | 98.4 |
| 4 | 1026 | 7800 | 4.0 | 0.78 | 98.6 |
The embodiment shows that the high-voltage-constant and high-density piezoelectric ceramic has large piezoelectric constant, dielectric constant and electromechanical coupling coefficient, high density and good uniformity, and is suitable for manufacturing piezoelectric actuator products requiring high deflection and piezoelectric sensor products requiring high sensitivity. The preparation method disclosed is simple and convenient to operate, high in yield and good in reliability, and the preparation conditions are easy to achieve, and the method is suitable for industrial production.
The foregoing description of the embodiments is provided to facilitate an understanding and appreciation of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications to the present invention based on the disclosure of the present invention within the protection scope of the present invention.
Claims (4)
1. A piezoelectric ceramic with high compactness and high piezoelectric constant has a chemical formula of Pb1-xMx(ZryTi1-y)0.75(Ni1/ 3Nb2/3)0.2(Sb1/3Nb2/3)0.015(Mg1/3Nb2/3)0.035O3+zwt%Bi2O3Wherein x is the sum of the elements in M, x = 0.07-0.15, y = 0.45-0.55, z = 0.2-1, and M is Ba2+、Sr2+、Ca2+、La3+One or a combination of more of the above; the preparation method of the high-density high-voltage constant piezoelectric ceramic comprises the following steps:
(1) adding Pb3O4、ZrO2、TiO2、NiO、Sb2O3、Nb2O5MgO, M and Bi2O3Preparing materials according to the stoichiometric ratio, and then mixing to obtain powder;
(2) preparing the required piezoelectric ceramic powder by ball milling, presintering, secondary ball milling and drying;
(3) adding deionized water and polyvinyl alcohol into the ceramic powder prepared in the step (2) according to a certain proportion for spray granulation;
(4) putting the ceramic powder prepared in the step (3) into a dry bag type cold isostatic press for pressing and molding to prepare the ceramic powder with the sintering density of more than or equal to 5.2g/cm3And testing the green density of the piezoelectric ceramic green body;
(5) keeping the green body at 550 ℃ for 4-6 hours to remove the glue, then heating to 1250-1300 ℃ at the speed of 3-5 ℃/min in the air atmosphere, and keeping the temperature for 2-4 hours to obtain the general formula Pb1-xMx(ZryTi1-y)0.75(Ni1/3Nb2/3)0.2(Sb1/3Nb2/3)0.015(Mg1/3Nb2/3)0.035O3+zwt%Bi2O3The piezoelectric ceramic of (1);
(6) the prepared piezoelectric ceramic is printed with silver and is polarized, and then the physical and electrical properties of the piezoelectric ceramic are tested.
2. The high-density high-piezoelectric-constant piezoelectric ceramic according to claim 1, wherein the pressure in step (4) is 60MPa to 120MPa, and the green compact density is 5.2g/cm3~5.5g/cm3Density uniformity of + -0.05 g/cm3。
3. The high-density high-piezoelectric-constant piezoelectric ceramic according to claim 1, wherein the sintered density of the piezoelectric ceramic of step (5) is greater than 98% of the theoretical density.
4. The piezoelectric ceramic with high density and high piezoelectric constant of claim 1, wherein the piezoelectric constant of the piezoelectric ceramic is 950 pC/N-1053 pC/N, and the electromechanical coupling coefficient is not less than 0.75.
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