CN115073159A - Bismuth ferrite-barium titanate ceramic with high Curie temperature and high piezoelectric performance and low-temperature oxygen-containing hot-pressing sintering preparation method thereof - Google Patents

Bismuth ferrite-barium titanate ceramic with high Curie temperature and high piezoelectric performance and low-temperature oxygen-containing hot-pressing sintering preparation method thereof Download PDF

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CN115073159A
CN115073159A CN202210912495.XA CN202210912495A CN115073159A CN 115073159 A CN115073159 A CN 115073159A CN 202210912495 A CN202210912495 A CN 202210912495A CN 115073159 A CN115073159 A CN 115073159A
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陈巧红
杨心怡
杨华斌
关士博
王雪婷
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Guilin University of Electronic Technology
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Abstract

The invention discloses bismuth ferrite-barium titanate ceramic with high Curie temperature and high piezoelectric property and a low-temperature oxygen-containing hot-pressing sintering preparation method thereof, wherein the general formula of the ceramic is as follows: (1-u)BiFeO 3uBaTiO 3 +1.0mol%MnCO 3 +xmol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 +ymol%Ba(W 1/2 Cu 1/2 )O 3 +zmol%B 2 O 3 Whereinu、xyAndzrepresents a molar fraction of (Bi) 0.5 Na 0.25 Li 0.25 )TiO 3 、Ba(W 0.5 Cu 0.5 )O 3 And B 2 O 3 Is a low-temperature sintering aid and is less than or equal to 0.20u≤0.45,0<x≤2.0,0≤y≤5.0,0≤zLess than or equal to 5.0. The method can be used for hot-pressing sintering at 820-920 ℃ and 25Mpa under the condition of oxygen-containing atmosphere by adding the sintering aid to obtain the porcelain. The invention reduces the sintering temperature of the bismuth ferrite-barium titanate ceramic, reduces the volatilization of Bi element, improves the density of the ceramic, reduces the dielectric loss of the ceramic and obtains the lead-free piezoelectric ceramic with high piezoelectric property, high Curie temperature and low dielectric loss.

Description

Bismuth ferrite-barium titanate ceramic with high Curie temperature and high piezoelectric performance and low-temperature oxygen-containing hot-pressing sintering preparation method thereof
Technical Field
The invention relates to a lead-free piezoelectric ceramic and a low-temperature hot-pressing sintering preparation technology, relates to bismuth ferrite-barium titanate ceramic, and particularly relates to bismuth ferrite-barium titanate ceramic with high Curie temperature and high piezoelectric performance and a low-temperature oxygen-containing hot-pressing sintering preparation method thereof.
Background
The piezoelectric ceramic is widely applied to the high-technology fields of aerospace, nuclear power, petrochemical industry, geological exploration, metallurgy, automobile fuel monitoring, 3D printing, high-temperature ultrasonic application and the like. At present, lead zirconate titanate (PZT) and a modified piezoelectric ceramic body thereof are mainly applied in the field, in order to save energy and reduce production cost, various sintering aids are adopted to reduce the sintering temperature of the ceramic, and meanwhile, the multilayer piezoelectric ceramic is expected to obtain lower sintering temperature in order to reduce the cost of an internal electrode. At present, the sintering temperature of a lead zirconate titanate system is reduced to about 950 ℃, but the problem of lead volatilization still exists in the process of sintering and preparing the multilayer piezoelectric ceramics at the temperature, and the environment is seriously polluted, so that the lead-free piezoelectric ceramics has important social significance.
BiFeO 3 -BaTiO 3 The ceramic has the excellent characteristics of high Curie temperature, low sintering temperature, no toxicity and perovskite structure, but in the sintering process, BiFeO is generated 3 With BaTiO 3 The sintering ceramic temperature difference is respectively 830 ℃ and 1400 ℃, and the ceramic is not enough and cannot be polarized when the sintering temperature is too low. When the sintering temperature is too high, the Bi element is seriously volatilized. In order to balance the valence, the volatilization of Bi element can cause a great deal of oxygen vacancy and lattice defect and hole in the ceramic, so thatThe dielectric loss of the system is very high and cannot be polarized, and after Mn element is added for doping modification, the resistivity of the system is effectively improved, the dielectric loss is reduced, but the dielectric loss is still higher (more than or equal to 5 percent), so that the BiFeO is reduced 3 -BaTiO 3 The dielectric loss of ceramics can be worked from the aspects of reducing sintering temperature and improving ceramic compactness.
The patent with publication number CN102584195A discloses a bismuth-based perovskite-type lead-free piezoelectric ceramic and a low-temperature preparation method thereof, wherein a solid-phase synthesis sintering method of adding a low-temperature sintering aid is adopted to successfully reduce the sintering temperature to about 900 ℃, but the problems of volatilization of bismuth and higher dielectric loss are still not solved.
Hot-pressing sintering is a common ceramic preparation method, however, because a high-temperature resistant hot-pressing mold is needed, hot-pressing sintering needs to be carried out under an oxygen-free protective atmosphere. In BiFeO 3 -BaTiO 3 During the preparation process of the system ceramic, the system is very easy to generate oxygen vacancy in the sintering process, so that the system cannot be sintered in an oxygen-free atmosphere.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides bismuth ferrite-barium titanate ceramic with high Curie temperature and high piezoelectric property and a low-temperature oxygen-containing hot-pressing sintering preparation method thereof to reduce BiFeO 3 -BaTiO 3 The sintering temperature of the system ceramic reduces the volatilization of Bi element, improves the Curie temperature and the high temperature stability of the system ceramic, and obtains BiFeO with high piezoelectric property, high Curie temperature and low dielectric loss 3 -BaTiO 3 A lead-free piezoelectric ceramic.
The technical scheme for realizing the purpose of the invention is as follows:
a bismuth ferrite-barium titanate ceramic having high Curie temperature and high piezoelectric properties, the ceramic having a general composition formula:
(1-u)BiFeO 3 -uBaTiO 3 +1.0mol%MnCO 3 +xmol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 +ymol%Ba(W 1/2 Cu 1/2 )O 3 +zmol%B 2 O 3 which isWherein u, x, y and z represent mole fractions, (Bi) 0.5 Na 0.25 Li 0.25 )TiO 3 、Ba(W 0.5 Cu 0.5 )O 3 And B 2 O 3 Is a low-temperature sintering aid, u is more than or equal to 0.20 and less than or equal to 0.45, x is more than 0 and less than or equal to 2.0, y is more than or equal to 0 and less than or equal to 5.0, and z is more than or equal to 0 and less than or equal to 5.0.
The low-temperature oxygen-containing hot-pressing sintering preparation method of the bismuth ferrite-barium titanate ceramic with high Curie temperature and high piezoelectric property comprises the following steps:
1) to analyze pure Fe 2 O 3 、Bi 2 O 3 、Li 2 CO 3 、Na 2 CO 3 、TiO 2 And nano BaTiO 3 The powder is used as a raw material according to (1-u) BiFeO 3 -uBaTiO 3 +xmol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 Burdening, wherein u is more than or equal to 0.20 and less than or equal to 0.45, x is more than 0 and less than or equal to 2.0, ball milling is carried out for 24 hours by taking absolute ethyl alcohol as a medium, drying is carried out for 12 hours at 100 ℃, sieving is carried out by a 250-mesh sieve of 200 meshes, the mixture is put into a high-aluminum crucible for compacting and covering, the temperature is increased to 750 ℃ at the heating rate of 250 ℃/h, and the mixture is kept warm for 6 hours for synthesis and standby;
2) to analytically pure BaCO 3 、WO 3 And CuO as raw materials, according to Ba (Cu) 1/2 W 1/2 )O 3 Proportioning materials in a chemical formula, mixing and ball-milling for 24h, taking out, drying, sieving by a 250-mesh sieve of 200 meshes, putting into a high-aluminum crucible, pressing and covering, heating to 850 ℃ at a heating rate of 250 ℃/h, and preserving heat for 6h for synthesis for later use;
3) the (1-u) BiFeO synthesized in the step 1) 3 -uBaTiO 3 +xmol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 And step 2) synthesized Ba (Cu) 1/2 W 1/2 )O 3 Powder and B 2 O 3 And MnCO 3 According to (1-u) BiFeO 3 -uBaTiO 3 +1.0mol%MnCO 3 +xmol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 +ymol%Ba(Cu 1/2 W 1/2 )O 3 +zmol%B 2 O 3 Mixing materials, wherein u is more than or equal to 0.20 and less than or equal to 0.45, x is more than 0 and less than or equal to 2.0, y is more than or equal to 0 and less than or equal to 5.0, and z is more than or equal to 0 and less than or equal to 5.0, taking absolute ethyl alcohol as a medium, taking out after ball milling for 24 hours, drying, and sieving with 200-mesh and 250-mesh sieveScreening for later use;
4) putting the powder synthesized in the step 3) into a hot-pressing sintering machine, adopting an alumina corundum mold, directly heating to 100 ℃ at the speed of 5 ℃/min under the condition of air or pure oxygen atmosphere, keeping the temperature for 15min to remove water vapor in the powder, quickly heating to 820-920 ℃ at the heating speed of 20 ℃/min, keeping the temperature unchanged, starting pressurizing to 25MPa, keeping the temperature and pressure for 30min, cutting off power, cooling with boiled water, and quickly cooling to room temperature;
5) cutting the sintered sample into ceramic wafers with different sizes according to requirements, polishing and processing the ceramic wafers into thin sheets with two smooth surfaces and the thickness of 0.5-1.0mm, and coating silver electrodes on the thin sheets;
6) and polarizing the fired piezoelectric ceramic plate in silicone oil, polarizing the piezoelectric ceramic plate in an electric field of 6000V/mm at 120 ℃, keeping the temperature for 30min, keeping the electric field and cooling to room temperature.
The invention adopts an alumina corundum mould and simultaneously adopts BiFeO 3 -BaTiO 3 Adding sintering aid Ba (W) into the powder 1/ 2 Cu 1/2 )O 3 、(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 、B 2 O 3 The sintering temperature is reduced, the system is hot-pressed and sintered under the condition of pure oxygen atmosphere or oxygen-containing atmosphere, the lowest hot-pressing sintering temperature is reduced to 820 ℃, and simultaneously (Bi) is utilized 0.5 Na 0.25 Li 0.25 )TiO 3 The low tolerance factor characteristic improves the Curie temperature and the high temperature stability of the system, and finally BiFeO with high piezoelectric property, high Curie temperature and low dielectric loss is obtained 3 -BaTiO 3 A lead-free piezoelectric ceramic.
The invention has the following positive effects:
(1) the technical proposal makes full use of Ba (Cu) 1/2 W 1/2 )O 3 And (Bi) 0.5 Na 0.25 Li 0.25 )TiO 3 Perovskite structure and low melting point characteristics of (1-u) BiFeO 3 -uBaTiO 3 Form good solid solution while adding B with low melting point 2 O 3 Low temperature liquid phase is formed in the sintering process, and the hot-pressing sintering temperature of the system is greatly reducedPromoting grain boundary movement and grain growth to 820 ℃, and obtaining the piezoelectric ceramic with uniform grain growth; on the other hand, (Bi) is fully utilized 0.5 Na 0.25 Li 0.25 )TiO 3 The Curie temperature and the high-temperature stability of the system are improved due to the characteristic of low tolerance factor;
(2) the hot-pressing sintering is carried out in a closed space, so that the volatilization of Bi element can be effectively prevented, the generation of holes and oxygen vacancies can be reduced, meanwhile, the density of the ceramic is improved by hot pressing, the lattice defect is reduced, and the dielectric loss of the ceramic is favorably reduced;
(3) the hot-pressing sintering is completed under the condition of oxygen-containing atmosphere, and BiFeO can be effectively avoided 3 -BaTiO 3 The ceramic is subjected to oxygen vacancy generation in the hot-pressing sintering process, and is subjected to water-cooling forced rapid cooling during cooling, so that the time of a cooling stage is reduced, and the generation of an intermediate phase is favorably reduced.
The invention successfully prepares (1-u) BiFeO by adding sintering aid and hot pressing process 3 -uBaTiO 3 +1.0mol%MnCO 3 The sintering temperature of the ceramic is reduced from 960 ℃ to 820-920 ℃, and the relative compactness of the system is improved from 95% to 99% while the sintering temperature is reduced, so that a piezoelectric ceramic sample with high Curie temperature, high piezoelectric performance and low dielectric loss is obtained, and the piezoelectric ceramic sample has excellent piezoelectric performance and high-temperature stability. The in-situ dynamic depolarization test result of the sample prepared in example 1 shows that, as shown in fig. 1, the piezoelectric ceramic prepared by the technology of the present invention has a use temperature range of more than 300 ℃, and the piezoelectric property of the piezoelectric ceramic reaches 498pC/N at a maximum temperature of 315 ℃.
Drawings
FIG. 1 is a graph showing the in-situ dynamic depolarization of the ceramic prepared in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings, in which the described examples are intended to illustrate only some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a bismuth ferrite-barium titanate ceramic having high curie temperature and high piezoelectric properties, the ceramic having the formula: 0.68BiFeO 3 -0.32BaTiO 3 +1.0mol%MnCO 3 +1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 +2.5mol%B 2 O 3 +3.0mol%Ba(Cu 1/2 W 1/2 )O 3
The low-temperature oxygen-containing hot-pressing sintering preparation method of the ceramic comprises the following steps:
(1) to analyze pure Fe 2 O 3 、Bi 2 O 3 、Li 2 CO 3 、Na 2 CO 3 、TiO 2 And nano BaTiO 3 The powder is used as a raw material according to 0.68BiFeO 3 -0.32BaTiO 3 +1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 Mixing materials, ball-milling for 24h by using absolute ethyl alcohol as a medium, taking out, drying at 100 ℃ for 12h, sieving by a 200-mesh sieve, putting into a high-aluminum crucible, compacting, covering, heating to 750 ℃ at a heating rate of 250 ℃/h, keeping the temperature for 6h, and synthesizing for later use;
(2) to analytically pure BaCO 3 、WO 3 And CuO as raw materials, according to Ba (Cu) 1/2 W 1/2 )O 3 Proportioning the materials according to the chemical formula, mixing and ball-milling for 24 hours, taking out, drying, sieving by a 200-mesh sieve, putting into a high-aluminum crucible, pressing and covering, heating to 850 ℃ at the heating rate of 250 ℃/h, and keeping the temperature for 6h to synthesize the materials for later use;
(3) 0.68BiFeO synthesized in the step (1) 3 -0.32BaTiO 3 +1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 And Ba (Cu) synthesized in the step (2) 1/2 W 1/2 )O 3 Powder and B 2 O 3 And MnCO 3 According to 0.68BiFeO 3 -0.32BaTiO 3 +1.0mol%MnCO 3 +1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 +3.0mol%Ba(Cu 1/2 W 1/2 )O 3 +2.5%B 2 O 3 Preparing materials, taking absolute ethyl alcohol as a medium, ball-milling for 24 hours, taking out, drying, and sieving by a 200-mesh sieve for later use;
(4) putting the powder synthesized in the step (3) into a hot-pressing sintering machine, adopting an alumina corundum mold, directly heating to 100 ℃ at a heating rate of 5 ℃/min under the condition of air or pure oxygen atmosphere, keeping the temperature for 15min to remove water vapor in the powder, heating to 880 ℃ at a heating rate of 20 ℃/min, keeping the temperature, gradually pressurizing to 25MPa, keeping the temperature and the pressure for 30min, then powering off, cooling with boiled water, and rapidly cooling to room temperature;
(5) cutting the sintered sample into ceramic wafers with different sizes according to requirements, polishing and processing the ceramic wafers into sheets with two smooth surfaces and a thickness of 1.0mm, wherein the sheets are coin-shaped or cuboid-shaped and are coated with silver electrodes;
(6) and polarizing the fired piezoelectric ceramic plate in silicone oil, polarizing the piezoelectric ceramic plate in an electric field of 6000V/mm at 120 ℃, keeping the temperature for 30min, keeping the electric field and cooling to room temperature.
The performance measurements are as follows:
d 33 (pC/N) Q m k p ε r Tanδ(%) T c (℃) T d (℃)
498 74 0.32 665 1.53 523 490
the in-situ dynamic depolarization test result of the sample prepared in the embodiment 1 shows that the piezoelectric ceramic prepared by the technology of the invention has the use temperature range of more than 300 ℃ and the piezoelectric performance of 498pC/N at the highest temperature point of 315 ℃ as shown in the attached figure 1.
Example 2:
a bismuth ferrite-barium titanate ceramic having high curie temperature and high piezoelectric properties, the ceramic having the formula: 0.70BiFeO 3 -0.30BaTiO 3 +1.0mol%MnCO 3 +2.0mol%Ba(Cu 1/2 W 1/2 )O 3 +2.5mol%B 2 O 3 +1.5mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3
The preparation method of the low-temperature oxygen-containing hot-pressing sintering ceramic is the same as that of the embodiment 1, except that the sintering temperature of the step (4) is 870 ℃.
The performance measurements are as follows:
d 33 (pC/N) Q m k p ε r Tanδ(%) T c (℃) T d (℃)
466 68 0.34 647 1.38 556 525
example 3:
a bismuth ferrite-barium titanate ceramic having high curie temperature and high piezoelectric properties, the ceramic having the formula: 0.65BiFeO 3 -0.35BaTiO 3 +1.0mol%MnCO 3 +1.0mol%Ba(Cu 1/2 W 1/2 )O 3 +2.5mol%B 2 O 3 +1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3
The preparation method of the low-temperature oxygen-containing hot-pressing sintering ceramic is the same as that of the embodiment 1, except that the sintering temperature in the step (4) is 920 ℃. The performance measurements are as follows:
d 33 (pC/N) Q m k p ε r Tanδ(%) T c (℃) T d (℃)
418 50 0.28 781 1.95 473 445
example 4:
a bismuth ferrite-barium titanate ceramic having high curie temperature and high piezoelectric properties, the ceramic having the formula: 0.75BiFeO 3 -0.25BaTiO 3 +1.0mol%MnCO 3 +2.0mol%Ba(Cu 1/2 W 1/2 )O 3 +1.0mol%B 2 O 3 +1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3
The preparation method of the low-temperature oxygen-containing hot-pressing sintering ceramic is the same as that in example 1, except that the sintering temperature in the step (4) is 820 ℃.
The performance measurements are as follows:
d 33 (pC/N) Q m k p ε r Tanδ(%) T c (℃) T d (℃)
407 39 0.31 583 0.96 590 545
the values of the upper and lower limits and the intervals of the components and the values of the upper and lower limits and the intervals of the process parameters listed in the above embodiments can all realize the invention, and the implementation is not always provided herein.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. The bismuth ferrite-barium titanate ceramic with high Curie temperature and high piezoelectric property is characterized in that the general formula of the ceramic is as follows:
(1-u)BiFeO 3 -uBaTiO 3 +1.0mol%MnCO 3 +xmol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 +
ymol%Ba(W 1/2 Cu 1/2 )O 3 +zmol%B 2 O 3 whereinu、xyAndzrepresents a molar fraction of (Bi) 0.5 Na 0.25 Li 0.25 )TiO 3 、Ba(W 0.5 Cu 0.5 )O 3 And B 2 O 3 Is a low-temperature sintering aid and is less than or equal to 0.20u≤0.45,0<x≤2.0,0≤y≤5.0,0≤z≤5.0。
2. The method for preparing bismuth ferrite-barium titanate ceramics with high Curie temperature and high piezoelectric property by low-temperature oxygen-containing hot-pressing sintering according to claim 1, which is characterized by comprising the following steps:
1) to analyze pure Fe 2 O 3 、Bi 2 O 3 、Li 2 CO 3 、Na 2 CO 3 、TiO 2 And nano BaTiO 3 The powder is used as a raw material according to
(1-u)BiFeO 3 -uBaTiO 3 +xmol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 The ingredients are mixed, wherein the content of the ingredients is more than or equal to 0.20u≤0.45,0<xBall milling is carried out for 24 hours by taking absolute ethyl alcohol as a medium, the ball milling is carried out for 12 hours after being taken out, the ball milling is dried for 12 hours at the temperature of 100 ℃, a 200-mesh and 250-mesh sieve is used for sieving, the ball milling is put into a high-alumina crucible for compacting and covering, the ball milling is heated to 750 ℃ at the heating rate of 250 ℃/h and is kept warm for 6 hours for synthesis and standby application;
2) to analytically pure BaCO 3 、WO 3 And CuO as raw materials, according to Ba (Cu) 1/2 W 1/2 )O 3 Proportioning materials in a chemical formula, mixing and ball-milling for 24h, taking out, drying, sieving by a 250-mesh sieve of 200 meshes, putting into a high-aluminum crucible, pressing and covering, heating to 850 ℃ at a heating rate of 250 ℃/h, and preserving heat for 6h for synthesis for later use;
3) the (1-u)BiFeO 3 -uBaTiO 3 +xmol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 And step 2) synthesized Ba (Cu) 1/2 W 1/2 )O 3 Powder and B 2 O 3 And MnCO 3 According to (1-u)BiFeO 3 -uBaTiO 3 +1.0mol%MnCO 3 + xmol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 +ymol%Ba(Cu 1/2 W 1/2 )O 3 +zmol%B 2 O 3 Mixing the materials, wherein the content of the mixture is more than or equal to 0.20u≤0.45,0<x≤2.0,0≤y≤5.0,0≤zNot more than 5.0, ball milling for 24h with absolute ethyl alcohol as medium, taking out, drying, sieving with 200-mesh sieve of 250 meshes for later use;
4) putting the powder synthesized in the step 3) into a hot-pressing sintering machine, adopting an alumina corundum mold, directly heating to 100 ℃ at the speed of 5 ℃/min under the condition of air or pure oxygen atmosphere, keeping the temperature for 15min to remove water vapor in the powder, quickly heating to 820-920 ℃ at the heating speed of 20 ℃/min, keeping the temperature unchanged, starting pressurizing to 25MPa, keeping the temperature and pressure for 30min, cutting off power, cooling with boiled water, and quickly cooling to room temperature;
5) cutting the sintered sample into ceramic wafers with different sizes according to requirements, polishing and processing the ceramic wafers into thin sheets with two smooth surfaces and the thickness of 0.5-1.0mm, and coating silver electrodes on the thin sheets;
6) and polarizing the fired piezoelectric ceramic plate in silicone oil, polarizing the piezoelectric ceramic plate in an electric field of 6000V/mm at 120 ℃, keeping the temperature for 30min, keeping the electric field and cooling to room temperature.
3. The bismuth ferrite-barium titanate ceramic having high curie temperature and high piezoelectric properties of claim 1, wherein the ceramic has a chemical formula of:
0.68BiFeO 3 -0.32BaTiO 3 +1.0mol%MnCO 3 +1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 +2.5mol%B 2 O 3 +
3.0mol%Ba(Cu 1/2 W 1/2 )O 3
4. the method for preparing bismuth ferrite-barium titanate ceramics with high Curie temperature and high piezoelectric property by low-temperature oxygen-containing hot-pressing sintering according to claim 3, which is characterized by comprising the following steps:
(1) to analyze pure Fe 2 O 3 、Bi 2 O 3 、Li 2 CO 3 、Na 2 CO 3 、TiO 2 And nano BaTiO 3 The powder is used as a raw material according to 0.68BiFeO 3 -0.32BaTiO 3 +1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 Mixing materials, ball-milling for 24h by using absolute ethyl alcohol as a medium, taking out, drying at 100 ℃ for 12h, sieving by a 200-mesh sieve, putting into a high-aluminum crucible, compacting, covering, heating to 750 ℃ at a heating rate of 250 ℃/h, keeping the temperature for 6h, and synthesizing for later use;
(2) to analytically pure BaCO 3 、WO 3 And CuO as raw materials, according to Ba (Cu) 1/2 W 1/2 )O 3 Proportioning the materials according to the chemical formula, mixing and ball-milling for 24 hours, taking out, drying, sieving by a 200-mesh sieve, putting into a high-aluminum crucible, pressing and covering, heating to 850 ℃ at the heating rate of 250 ℃/h, and keeping the temperature for 6h to synthesize the materials for later use;
(3) 0.68BiFeO synthesized in the step (1) 3 -0.32BaTiO 3 +1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 And Ba (Cu) synthesized in step (2) 1/2 W 1/2 )O 3 Powder and B 2 O 3 And MnCO 3 According to 0.68BiFeO 3 -0.32BaTiO 3 + 1.0mol%MnCO 3 +1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3 +3.0mol%Ba(Cu 1/2 W 1/2 )O 3 +2.5%B 2 O 3 Preparing materials, taking absolute ethyl alcohol as a medium, ball-milling for 24 hours, taking out, drying, and sieving by a 200-mesh sieve for later use;
(4) putting the powder synthesized in the step (3) into a hot-pressing sintering machine, adopting an alumina corundum mold, directly heating to 100 ℃ at the heating rate of 5 ℃/min under the condition of air or pure oxygen atmosphere, keeping the temperature for 15min to remove water vapor in the powder, heating to 880 ℃ at the heating rate of 20 ℃/min, keeping the temperature, gradually pressurizing to 25Mpa, keeping the temperature and the pressure for 30min, then powering off, cooling with boiled water, and rapidly cooling to room temperature;
(5) cutting the sintered sample into ceramic wafers with different sizes according to requirements, polishing and processing the ceramic wafers into sheets with two smooth surfaces and a thickness of 1.0mm, wherein the sheets are coin-shaped or cuboid-shaped and are coated with silver electrodes;
(6) and polarizing the fired piezoelectric ceramic plate in silicone oil, polarizing the piezoelectric ceramic plate in an electric field of 6000V/mm at 120 ℃, keeping the temperature for 30min, keeping the electric field and cooling to room temperature.
5. The bismuth ferrite-barium titanate ceramic having high curie temperature and high piezoelectric properties of claim 1, wherein the ceramic has a chemical formula of:
0.70BiFeO 3 -0.30BaTiO 3 +1.0mol%MnCO 3 +2.0mol%Ba(Cu 1/2 W 1/2 )O 3 +2.5mol%B 2 O 3 +
1.5mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3
6. the bismuth ferrite-barium titanate ceramic having high curie temperature and high piezoelectric properties of claim 1, wherein the ceramic has a chemical formula of:
0.65BiFeO 3 -0.35BaTiO 3 +1.0mol%MnCO 3 +1.0mol%Ba(Cu 1/2 W 1/2 )O 3 +2.5mol%B 2 O 3 +
1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3
7. the bismuth ferrite-barium titanate ceramic having high curie temperature and high piezoelectric properties of claim 1, wherein the ceramic has a chemical formula of:
0.75BiFeO 3 -0.25BaTiO 3 +1.0mol%MnCO 3 +2.0mol%Ba(Cu 1/2 W 1/2 )O 3 +1.0mol%B 2 O 3 +
1.0mol%(Bi 0.5 Na 0.25 Li 0.25 )TiO 3
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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1541978A (en) * 2003-11-07 2004-11-03 ���Ĵ���ѧ Bismuth sodium lithium titanate barium titanate strontium titanate calcium titanate based lead-free piezoelectric ceramics
JP2007031219A (en) * 2005-07-28 2007-02-08 Toyota Motor Corp Bismuth sodium titanate-barium zirconium titanate base lead-free piezoelectric ceramic and its producing method
WO2008078703A1 (en) * 2006-12-25 2008-07-03 Kyocera Corporation Piezoelectric ceramic and piezoelectric element
US20090267016A1 (en) * 2005-10-27 2009-10-29 Kyocera Corporation Piezoelectric ceramic composition and piezoelectric ceramic
CN104387049A (en) * 2014-11-27 2015-03-04 桂林电子科技大学 Leadless piezoelectric ceramic and method for preparing leadless piezoelectric ceramic by virtue of low-temperature liquid phase sintering
JP2015130505A (en) * 2013-06-28 2015-07-16 セイコーエプソン株式会社 Method for manufacturing piezoelectric material, piezoelectric element, liquid ejecting head, liquid ejecting apparatus, ultrasonic sensor, piezoelectric motor, and power generator
CN110128127A (en) * 2019-07-01 2019-08-16 桂林电子科技大学 A kind of bismuth ferrite with high tension performance and high-temperature stability-barium titanate-based lead-free piezoelectric ceramics and preparation method thereof
CN110128128A (en) * 2019-07-01 2019-08-16 桂林电子科技大学 A kind of bismuth ferrite-bismuth aluminate with zero-temperature coefficient and high-temperature stability-zinc bismuth titanates high-temperature piezoelectric ceramics and preparation method thereof
CN110128126A (en) * 2019-07-01 2019-08-16 桂林电子科技大学 A kind of bismuth ferrite-metatitanic acid barium-zinc bismuth titanates-bismuth aluminate high-temp leadless piezoelectric ceramics and preparation method thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1541978A (en) * 2003-11-07 2004-11-03 ���Ĵ���ѧ Bismuth sodium lithium titanate barium titanate strontium titanate calcium titanate based lead-free piezoelectric ceramics
JP2007031219A (en) * 2005-07-28 2007-02-08 Toyota Motor Corp Bismuth sodium titanate-barium zirconium titanate base lead-free piezoelectric ceramic and its producing method
US20090267016A1 (en) * 2005-10-27 2009-10-29 Kyocera Corporation Piezoelectric ceramic composition and piezoelectric ceramic
WO2008078703A1 (en) * 2006-12-25 2008-07-03 Kyocera Corporation Piezoelectric ceramic and piezoelectric element
JP2015130505A (en) * 2013-06-28 2015-07-16 セイコーエプソン株式会社 Method for manufacturing piezoelectric material, piezoelectric element, liquid ejecting head, liquid ejecting apparatus, ultrasonic sensor, piezoelectric motor, and power generator
CN104387049A (en) * 2014-11-27 2015-03-04 桂林电子科技大学 Leadless piezoelectric ceramic and method for preparing leadless piezoelectric ceramic by virtue of low-temperature liquid phase sintering
CN110128127A (en) * 2019-07-01 2019-08-16 桂林电子科技大学 A kind of bismuth ferrite with high tension performance and high-temperature stability-barium titanate-based lead-free piezoelectric ceramics and preparation method thereof
CN110128128A (en) * 2019-07-01 2019-08-16 桂林电子科技大学 A kind of bismuth ferrite-bismuth aluminate with zero-temperature coefficient and high-temperature stability-zinc bismuth titanates high-temperature piezoelectric ceramics and preparation method thereof
CN110128126A (en) * 2019-07-01 2019-08-16 桂林电子科技大学 A kind of bismuth ferrite-metatitanic acid barium-zinc bismuth titanates-bismuth aluminate high-temp leadless piezoelectric ceramics and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
YING LI 等: ""Enhancement in multiferroic and piezoelectric properties of BiFeO3–BaTiO3–Bi0.5Na0.5TiO3 lead-free ceramics with MnO2 addition by optimizing sintering temperature and dwell time"", pages 92 - 99 *

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