CN114292102B - Bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material and preparation method thereof - Google Patents
Bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material and a preparation method thereof. The chemical composition of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material is xBiFeO 3 ‑yBaTiO 3 ‑zBi(Mg 0.5 Hf 0.5 )O 3 (ii) a Wherein x + y + z =1, x =0.6 to 0.85, y =0.15 to 0.35, and z =0 to 0.05.
Description
Technical Field
The invention relates to a high-Curie temperature, high-resistivity and large-electrical-strain bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic and a preparation method thereof, belonging to the field of lead-free piezoelectric ceramic materials.
Background
Based on the characteristic that piezoelectric ceramics can realize the interconversion of electrical signals and mechanical strain, the piezoelectric ceramics can be made into devices such as sensors, piezoelectric transducers, drivers and the like, can be widely applied to the fields of aerospace, underwater acoustic detection, nondestructive testing and the like, but at some extreme endsWhen applied in environments, such as high temperature and high pressure environments, higher performance requirements are imposed on piezoelectric ceramic materials. At present, the high-temperature piezoelectric ceramics mainly comprise four major types of tungsten bronze structures, perovskite structures, bismuth layer structures, perovskite-like structures and the like. Bismuth ferrite (BiFeO) 3 ) The high-temperature piezoelectric ceramic belongs to perovskite, and has higher Curie temperature and high piezoelectric performance compared with other three types. But BiFeO 3 The higher leakage current and lower high temperature resistivity limit their applications. BiFeO is prepared 3 Barium titanate (BaTiO) 3 ) The binary system after compounding can well reduce the leakage current of the material and improve the piezoelectric performance, but the Curie temperature is reduced along with the reduction of the material. How to balance the relationship among Curie temperature, high-temperature resistivity and piezoelectric performance, obtain components with excellent performance and meet the requirements of production and application is a key problem to be solved urgently.
Generally, in a ferroelectric material, a relaxor ferroelectric is solid-solution, and a ferroelectric to relaxor ferroelectric transition occurs, and the transition component thereof is called a second type of morphotropic phase boundary. While ferroelectric relaxor ceramic materials in this range tend to exhibit excellent piezoelectric properties, for example, lead magnesium niobate (PMN) can achieve large electrostriction in lead zirconate titanate (PZT). In the relaxor ferroelectric material, the relaxation degree of Bismuth Magnesium Hafnium (BMH) is stronger than that of common relaxor ferroelectrics such as Bismuth Magnesium Titanate (BMT) and Bismuth Magnesium Zirconium (BMZ). BMH is compounded in bismuth ferrite-barium titanate (BF-BT), and the proportion of BF and BT is adjusted, so that a transition component from ferroelectric to relaxor ferroelectric can be obtained, and the lead-free piezoelectric ceramic material with high Curie temperature, large electrostriction and high resistivity is obtained.
Disclosure of Invention
In order to obtain high Curie temperature, high resistivity and large strain value in the lead-free piezoelectric ceramic material at the same time, the invention provides the bismuth ferrite-barium titanate ceramic material of the solid solution hafnium magnesium acid bismuth with high Curie temperature, high resistivity and large strain and the preparation method thereof.
On one hand, the invention provides a bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material, and the chemical composition of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material is xBiFeO 3 -yBaTiO 3 -zBi(Mg 0.5 Hf 0.5 )O 3 (ii) a Wherein x + y + z =1, x =0.6 to 0.85, y =0.15 to 0.35, and z =0 to 0.05.
The invention has the key points that the ratio of bismuth ferrite to barium titanate is adjusted to reduce leakage current and improve resistivity, and the inventor shows through research that the resistivity can be improved by reducing the content of bismuth ferrite in a formula and the electrical-relaxation phase transition of iron is generated. On the basis, hafnium-magnesium Bismuth (BMH) with high relaxation degree is further selected for doping, the disorder degree of the components is increased, the ferroelectric-relaxation phase transition is completed on the premise of ensuring higher Curie temperature, and the relaxation ferroelectric ceramic material with large strain value is obtained.
Preferably, y = 0.25-0.35, z =0.05.
Preferably, the resistivity of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material at 300 ℃ is more than 10 4 Preferably > 10 6 。
Preferably, the Curie temperature of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material is more than 300 ℃.
Preferably, the electrical strain of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material is more than or equal to 0.02 percent, and preferably more than 2 percent.
On the other hand, the invention provides a preparation method of the bismuth ferrite-barium titanate-based piezoelectric ceramic material, which uses Fe 2 O 3 、Bi 2 O 3 、BaCO 3 、TiO 2 、MgO、HfO 2 The powder is taken as a raw material, and the chemical composition of the bismuth ferrite-barium titanate based lead-free piezoceramic material xBiFeO is adopted 3 -yBaTiO 3 -zBi(Mg 0.5 Hf 0.5 )O 3 And (3) carrying out material mixing, synthesis, fine grinding, granulation, molding, plastic discharge and sintering to obtain the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material.
Preferably, the mixing and fine grinding mode is wet ball milling; wherein, the raw materials: ball milling medium: the mass ratio of the deionized water =1: (1.6-2.4): (0.8-1.2) and performing planetary ball milling mixing for 2-6 hours at the rotating speed of 300-400 rpm, wherein the ball milling medium is agate balls.
Preferably, the synthesis temperature is 700-850 ℃, and the synthesis time is 4-6 hours; preferably, the heating rate of the synthesis is 4-6 ℃/min.
Preferably, a binder accounting for 5-10% of the mass of the synthesized ceramic powder is added in the granulation process for granulation; preferably, the binder is a polyvinyl alcohol solution with a concentration of 4 to 8 wt.%.
Preferably, the temperature of the plastic discharge is 600-800 ℃, and the heat is preserved for 3 hours; preferably, the temperature rise rate of the plastic discharge is not higher than 2 ℃/min.
Preferably, the sintering temperature is 980-1030 ℃ and the sintering time is 2-5 hours.
Preferably, the obtained bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material is subjected to electrode preparation; preferably, the electrode is a silver paste electrode, the sintering condition of the electrode is 700-800 ℃, and the temperature is kept for less than 60 minutes.
Has the beneficial effects that:
in the present invention, the resistivity can be increased by reducing the bismuth ferrite content in the formulation, and a pig iron electro-relaxation phase transition occurs. On the basis, hafnium magnesium bismuth acid (BMH) with high relaxation degree is further selected for doping, the disorder degree of the components is increased, the ferroelectric-relaxation phase transition is completed on the premise of ensuring higher Curie temperature, and the relaxation ferroelectric ceramic material with large strain value is obtained. Specifically, the traditional solid phase hair preparation method is adopted to obtain the solid phase hair dye with Curie temperature of more than 300 ℃ and resistivity of more than 10 at 300 DEG C 6 And a piezoelectric ceramic having a large strain characteristic. The piezoelectric ceramic material has the characteristics of high Curie temperature, high resistivity and large strain value, and is suitable for being used as a high-temperature driver material.
Drawings
FIGS. 1a to 1d are dielectric thermograms of bismuth ferrite-barium titanate-based lead-free piezoelectric ceramics prepared in examples 1 to 4, respectively;
FIGS. 2a to 2d are the hysteresis loop and the strain, respectively, of the bismuth ferrite-barium titanate-based lead-free and lead-free piezoelectric ceramics prepared in examples 1 to 4;
FIG. 3 is a graph showing the temperature swing resistivity of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramics prepared in examples 1 to 4;
fig. 4 is a hysteresis loop and strain of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramics prepared in example 5, example 6 and example 7;
FIG. 5 is a graph showing the hysteresis loop and strain of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic prepared in comparative examples 1 to 2;
FIG. 6 is a graph showing the temperature change resistivity of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramics according to comparative examples 1 to 2.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the field, the bismuth ferrite-based ceramic material has very high electric leakage due to high-temperature bismuth ion volatilization and iron ion valence change, and the high-temperature low resistivity limits the further application of the bismuth ferrite-based ceramic material. The introduction of barium titanate can reduce the content of iron element in the formula, reduce leakage current and improve resistivity. However, the Curie temperature is also reduced due to the reduction of the content of bismuth ferrite, so that the search for an optimal composition with high Curie temperature and high resistivity is very important.
To this end, the inventors inventively: during the process of reducing the bismuth ferrite content and increasing the barium titanate content, the composition undergoes a phase transition from ferroelectric to relaxative transition. Meanwhile, the relaxation ferroelectric material bismuth magnesium hafnium oxide can be doped, so that the disorder degree of the material can be further improved, the activation energy of domain deflection is reduced, the ferroelectric-relaxation phase transition is completed on the premise of ensuring high Curie temperature, and excellent electrostriction performance is obtained.
In the invention, the chemical composition of the lead-free piezoceramic material with high Curie temperature, high resistivity and large strain is xBiFeO 3 -yBaTiO 3 -zBi(Mg 0.5 Hf 0.5 )O 3 Wherein x + y + z =1, x =0.6 to 0.85, y =0.15 to 0.35, y =0 to 0.05, preferably x =0.6 to 0.7, y =0.25 to 0.35, and z =0.05. If the value of y is lower, the piezoelectric ceramic resistance is lower; if the y content is too high, the pressure is increasedThe electroceramic full relaxation strain is reduced. If the value of z is low, the strain will not be significantly increased; if the z content is too high, the material will relax completely and lose the piezoelectric performance.
In an alternative embodiment, the lead-free piezoelectric ceramic has a curie temperature greater than 300 ℃; the electrical strain of the leadless piezoelectric ceramic is at least 0.03%, preferably 0.16-0.24%; the lead-free piezoelectric ceramic material has a resistivity of at least 5.4 x 10 at 300 DEG C 4 Preferably 5.7X 10 5 ～3.8×10 6 。
In one embodiment of the invention, the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material with high Curie temperature, high resistivity and large electrostrictive strain is prepared by adopting a traditional solid-phase method, the preparation method is simple, easy to popularize and wide in prospect, and the preparation method specifically comprises the steps of material mixing, synthesis, fine grinding, granulation, molding, plastic discharge, sintering and electrode preparation, and is provided by the invention. The following is an exemplary preparation method of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material.
Preparing ceramic powder by a solid phase method. With Fe 2 O 3 、Bi 2 O 3 、BaCO 3 、TiO 2 、MgO、HfO 2 The powder is used as a raw material, is prepared according to a stoichiometric ratio, is mixed and dried to obtain a dried raw material (namely mixed powder). Briquetting the dried raw materials, synthesizing in an alumina crucible by a solid phase method, heating to 700-850 ℃ at a heating rate of 4-6 ℃/min, preserving heat, synthesizing for 4-6 hours to obtain ceramic powder, and cooling to room temperature along with the furnace temperature to obtain the ceramic powder.
The ceramic powder is mechanically crushed, finely ground and dried to obtain the synthetic powder. Preferably, the fine grinding conditions and mode are consistent with the mixing.
Adding a binder accounting for 5 to 10 percent of the mass of the synthetic powder for grinding and granulating. Preferably, the binder is a polyvinyl alcohol solution of 4 to 8 wt.%.
The powder was pressed into green compacts using simple mechanical compression. Preferably, the molding pressure is 1 to 2MPa. Preferably, the blank size is diameter (12-14 mm) and thickness (1-2 mm). Heating the green body to 600-800 ℃ at a heating rate of not higher than 2 ℃/min, and preserving heat for less than 3 hours to carry out plastic removal treatment.
And placing the green body after plastic removal into a crucible, sintering for 2-5 hours at 980-1030 ℃, and cooling to room temperature along with the furnace temperature to obtain the bismuth ferrite-barium titanate piezoelectric ceramic. Preparing an electrode on the surface of the ceramic by screen printing, and sintering at 700-800 ℃ for less than 60min, wherein the electrode is preferably a platinum electrode.
The bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material prepared by the method has the characteristics of high Curie temperature, high resistivity and large electrostrictive strain, and can be widely applied to drivers and displacement brakes.
The present invention will be described in further detail with reference to examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing description are intended to be included within the scope of the invention. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
The preparation component is 0.8BiFeO 3 -0.15BaTiO 3 -0.05Bi(Mg 0.5 Hf 0.5 )O 3 The preparation method of the lead-free piezoelectric ceramic material comprises the following steps:
to analytically pure BaCO 3 、TiO 2 、Bi 2 O 3 、Fe 2 O 3 、MgO、HfO 2 The raw materials are mixed and blended according to the target chemical composition, and are uniformly mixed and dried by adopting wet ball milling, wherein the raw materials comprise the following components in percentage by weight: agate ball: deionized water =1:2:0.6 to 0.8, and the mixture is subjected to planetary ball milling for 4 to 6 hours. Drying at 100 ℃, sieving with a 40-mesh sieve, and molding under the pressure of 3 MPa. Then placing the mixture in an alumina crucible and synthesizing the mixture by a solid phase method, heating the mixture to 800 ℃ at the speed of 5 ℃/min, preserving the heat for 5 hours, and cooling the mixture to room temperature along with the furnace temperature. Mechanically pulverizing the synthetic raw material, and sieving with 40 mesh sieveAnd then, fine grinding is carried out by adopting the same process of mixing materials. Then adding a binder (polyvinyl alcohol PVA) accounting for 6% of the mass of the synthetic powder for granulation, forming under the pressure of 5MPa, aging for 24 hours, sieving by a 40-mesh sieve, and pressing under the pressure of 200MPa to prepare a green body. Heating the green body to 650 ℃ at the speed of 2 ℃/min, and preserving heat for 2 hours for plastic removal. After plastic removal, heating to 1000 ℃ at a speed of 5 ℃/min, keeping the temperature for 200min, sintering, and cooling to room temperature along with the furnace to obtain the lead-free piezoelectric ceramic material. And processing and cleaning the obtained ceramic chip, preparing a double-sided silver paste electrode by screen printing, raising the temperature to 750 ℃ at the heating rate of 5 ℃/min, and preserving heat for 30 minutes for sintering.
The dielectric temperature spectrum, the hysteresis loop and the strain loop spectrum, and the temperature-change resistivity of the lead-free piezoelectric ceramic material prepared in this example 1 are shown in fig. 1, fig. 2 and fig. 3, respectively. The lead-free piezoelectric ceramic material has Curie temperature of 653 deg.c, electric strain of 0.03% and resistivity of 5.4 x 10 at 300 deg.c 4 Ω·cm。
Example 2
The preparation component is 0.75BiFeO 3 -0.2BaTiO 3 -0.05Bi(Mg 0.5 Hf 0.5 )O 3 The lead-free piezoelectric ceramic of (1) was prepared in the same manner as in example 1.
The dielectric temperature spectrum, the hysteresis loop, the strain loop and the temperature-change resistivity of the lead-free piezoelectric ceramic material prepared in this example 2 are shown in fig. 1, fig. 2 and fig. 3, respectively. The obtained lead-free piezoelectric ceramic has Curie temperature of 630 deg.C, electrostriction of 0.06%, resistivity of 1 × 10 at 300 deg.C 5 Ω·cm。
Example 3
The preparation component is 0.7BiFeO 3 -0.25BaTiO 3 -0.05Bi(Mg 0.5 Hf 0.5 )O 3 The lead-free piezoelectric ceramic of (4) was prepared in the same manner as in example 1.
The dielectric temperature spectrum, the electrical hysteresis loop, the strain loop and the temperature-change resistivity of the lead-free piezoelectric ceramic material prepared in this example 3 are respectively shown in fig. 1, fig. 2 and fig. 3. The obtained leadless piezoelectric ceramic has Curie temperature of 616 deg.C, electrostriction of 0.16%, and resistivity of 5.7 × 10 at 300 deg.C 5 Ω·cm。
Example 4
The preparation component is 0.6BiFeO 3 -0.35BaTiO 3 -0.05Bi(Mg 0.5 Hf 0.5 )O 3 The lead-free piezoelectric ceramic of (4) was prepared in the same manner as in example 1.
The dielectric temperature spectrum, the electrical hysteresis loop, the strain loop and the temperature-change resistivity of the lead-free piezoelectric ceramic material prepared in this example 4 are respectively shown in fig. 1, fig. 2 and fig. 3. The obtained lead-free piezoelectric ceramic has Curie temperature of 350 deg.C, electrostriction of 0.24%, and resistivity of 3.8 × 10 at 300 deg.C 6 Omega cm, the resistivity and the electrostrictive strain are remarkably improved compared with the piezoelectric ceramics prepared in the examples 1 to 3 and the comparative example 1.
Example 5
The preparation component is 0.693BiFeO 3 -0.297BaTiO 3 -0.01Bi(Mg0 .5 Hf 0.5 )O 3 The lead-free piezoelectric ceramic of (1) was prepared in the same manner as in example 1.
The hysteresis loop and the strain loop 4a of the lead-free piezoelectric ceramic material prepared in this example 5 are shown. The electrical strain of the obtained lead-free piezoelectric ceramic is 0.17%, and compared with the piezoelectric ceramic prepared in examples 6 and 7 and the piezoelectric ceramic prepared in comparative example 2, the electrical strain is obviously improved, which shows that the electrical strain of the material can be improved by doping a proper amount of BMH. But the electrostrictive strain was small as compared with the piezoelectric ceramic prepared in example 4.
Example 6
The preparation component is 0.686BiFeO 3 -0.294BaTiO 3 -0.02Bi(Mg0 .5 Hf 0.5 )O 3 The lead-free piezoelectric ceramic of (4) was prepared in the same manner as in example 1.
The hysteresis loop and the strain loop 4b of the lead-free piezoelectric ceramic material prepared in this example 6 are shown. The electrical strain of the obtained lead-free piezoelectric ceramic is 0.16%, and compared with the piezoelectric ceramic prepared in the comparative example 2, the electrical strain is obviously improved.
Example 7
The preparation component is 0.679BiFeO 3 -0.291BaTiO 3 -0.03Bi(Mg0 .5 Hf 0.5 )O 3 The lead-free piezoelectric ceramic of (4) was prepared in the same manner as in example 1.
The hysteresis loop and the strain loop 4c of the lead-free piezoelectric ceramic material prepared in this example 7 are shown. The electrical strain of the obtained lead-free piezoelectric ceramic is 0.14%, and compared with the piezoelectric ceramic prepared in the comparative example 2, the electrical strain is slightly improved.
Comparative example 1
The preparation component is 0.75BiFeO 3 -0.25BaTiO 3 The preparation method of the piezoelectric ceramic material undoped with BMH is the same as that of example 1. The electrical return and strain are shown in figure 5 a.
Comparative example 2
The preparation component is 0.7BiFeO 3 -0.3BaTiO 3 The BMH undoped piezoelectric ceramic material was prepared in the same manner as in example 1, and the hysteresis loop and strain are shown in FIG. 5 b.
Table 1 shows the composition and performance parameters of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material:
the temperature-variable resistivity data is obtained by combining a German Novocontrol Technologies impedance Analyzer with Novotherm-HT, the electric loop and the strain are obtained by adopting a German TF Analyzer2000 ferroelectric Analyzer, and the dielectric temperature data is obtained by connecting an Agilent precision impedance Analyzer with a GJW-1 high-temperature dielectric temperature spectrum testing system.
Claims (14)
1. The bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material is characterized in that the chemical composition of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material is xBiFeO 3 -yBaTiO 3 -zBi(Mg 0.5 Hf 0.5 )O 3 (ii) a Wherein, x + y + z =1, x = 0.6-0.85, y = 0.15-0.35, z is more than 0 and less than or equal to 0.05;
the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material has the resistivity of more than 10 at 300 DEG C 4 ；
The Curie temperature of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material is more than 300 ℃;
the electro-strain of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material is more than or equal to 0.02 percent.
2. The bismuth-barium ferrite-titanate-based lead-free piezoelectric ceramic material according to claim 1, wherein y = 0.25-0.35.
3. The bismuth iron-barium titanate-based lead-free piezoelectric ceramic material according to claim 1, wherein the resistivity of the bismuth iron-barium titanate-based lead-free piezoelectric ceramic material at 300 ℃ is greater than 10 6 ；
The electrical strain of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material is more than 2 percent.
4. A method for preparing a bismuth ferrite-barium titanate-based piezoelectric ceramic material according to any one of claims 1 to 3, wherein Fe is used 2 O 3 、Bi 2 O 3 、BaCO 3 、TiO 2 、MgO、HfO 2 The powder is used as a raw material, and the chemical composition (0.95-x-y) BiFeO of the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material is adopted 3 -xBaTiO 3 -yBi(Mg 0.5 Hf 0.5 )O 3 And (3) carrying out material mixing, synthesis, fine grinding, granulation, molding, plastic discharge and sintering to obtain the bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic material.
5. The preparation method according to claim 4, characterized in that the mixing and fine grinding are performed by wet ball milling; wherein, the raw materials: ball milling medium: the mass ratio of the deionized water =1: (1.6-2.4): (0.8-1.2), and the mixture is subjected to planetary ball milling for 2-6 hours at the rotating speed of 300-400 rpm; wherein, the ball milling medium is agate balls.
6. The method of claim 4, wherein the synthesis is carried out at a temperature of 700 to 850 ℃ for a period of 4 to 6 hours.
7. The method according to claim 6, wherein the synthesis is carried out at a temperature increase rate of 4 to 6 ℃/min.
8. The preparation method according to claim 4, wherein a binder in an amount of 5-10% by mass of the synthesized ceramic powder is added during the granulation process to granulate.
9. The method of claim 8, wherein the binder is a polyvinyl alcohol solution having a concentration of 4 to 8 wt.%.
10. The preparation method of claim 4, wherein the temperature of the plastic discharge is 600-800 ℃, and the temperature is kept for 3 hours.
11. The method of claim 10, wherein the rate of temperature increase of the plastic discharge is not higher than 2 ℃/min.
12. The method according to claim 4, wherein the sintering temperature is 980-1030 ℃ and the sintering time is 2-5 hours.
13. The production method according to any one of claims 4 to 12, wherein the obtained bismuth-barium ferrite-barium titanate-based lead-free piezoelectric ceramic material is subjected to electrode fabrication.
14. The preparation method of claim 13, wherein the electrode is a silver paste electrode, and the sintering condition of the electrode is 700-800 ℃ and the temperature is kept for less than 60 minutes.
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