CN114920553A - Manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic and preparation method and application thereof - Google Patents
Manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic and preparation method and application thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 81
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910002115 bismuth titanate Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 20
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 20
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 19
- 239000011591 potassium Substances 0.000 claims abstract description 19
- 239000011734 sodium Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000010287 polarization Effects 0.000 claims abstract description 9
- 239000000853 adhesive Substances 0.000 claims abstract description 7
- 230000001070 adhesive effect Effects 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010931 gold Substances 0.000 claims abstract description 6
- 229910052737 gold Inorganic materials 0.000 claims abstract description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000007747 plating Methods 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000003825 pressing Methods 0.000 claims abstract description 3
- 230000028161 membrane depolarization Effects 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 10
- 230000005684 electric field Effects 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 241000764238 Isis Species 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 abstract 1
- 239000011572 manganese Substances 0.000 description 15
- 229910052748 manganese Inorganic materials 0.000 description 9
- 235000012431 wafers Nutrition 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000000227 grinding Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 239000012467 final product Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000011363 dried mixture Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000026683 transduction Effects 0.000 description 1
- 238000010361 transduction Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
The invention provides manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic and a preparation method and application thereof. The preparation method comprises the following steps: adding Bi 2 O 3 、Na 2 CO 3 、K 2 CO 3 、BaCO 3 、TiO 2 And MnO 2 Mixing, adding absolute ethyl alcohol, ball-milling, drying, and calcining to obtain pre-sintered powder with a perovskite structure; adding anhydrous ethyl to presintering powder with perovskite structureAlcohol ball milling, drying and pressing forming; discharging the adhesive at 500-650 ℃ for 2-4 h, sintering at 1150-1200 ℃, and keeping the temperature for 2-3h, wherein the heating rate is 2-3 ℃/min, and the cooling rate is 4-5 ℃/min, so as to obtain the manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate ceramic wafer; and plating gold on the sintered ceramic wafer for 10-20 min, and carrying out polarization treatment to obtain the manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic. The manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic prepared by the preparation method can be used for piezoelectric devices.
Description
Technical Field
The invention belongs to the technical field of piezoelectric materials, relates to manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramics, and particularly relates to manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramics, and a preparation method and application thereof, wherein the manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramics has high piezoelectricity and high temperature stability.
Background
Piezoelectric ceramics, as a functional material capable of converting mechanical energy and electric energy into each other, has very important application in driving, sensing and transduction, and occupies a great position in national economy and national safety fields such as information technology, photoelectron technology, precise control technology, nondestructive detection technology, electroacoustic technology, tuning technology and the like. In recent years, with the improvement of ecological environment awareness and the implementation of social sustainable development strategy, the production and use of lead-based piezoelectric ceramics and related devices are limited, and the research and development and use of lead-free piezoelectric ferroelectric ceramics are carried out at the same time.
At present, perovskite type lead-free piezoelectric systems mainly comprise barium titanate, potassium sodium niobate, bismuth sodium titanate and bismuth ferrite. Wherein, sodium bismuth titanate (Bi) 0.5 Na 0.5 TiO 3 BNT) has not only good electromechanical properties but also a curie temperature (Tm-300 ℃) comparable to that of lead-based ceramics as an a-site composite perovskite structure solid solution, and is considered as one of materials expected to replace lead-based piezoelectric ceramics. In addition, the highly disordered structure and complex phase transition of the BNT-based ceramic mean that the system may have abundant new phenomena, new rules, new performances and new applications to be further explored. In conclusion, the BNT-based ceramic not only has the potential of practical development, but also has more scientific research value due to the unique structure and properties of the material.
The existence of ferroelectric-relaxation phase transition of the bismuth sodium titanate-based piezoelectric ceramic causes the depolarization phenomenon to exist before the Curie temperature, and the piezoelectric performance is rapidly degraded near the temperature, so that the temperature (depolarization temperature, Td) is the key for limiting the temperature application range. At present, generalThe piezoelectric coefficient d can be effectively improved by methods such as chemical modification (including introduction of different elements, construction of a multi-element system and doping of oxides), process regulation (quenching) and the like 33 And a depolarization temperature Td. However, the piezoelectric coefficient d of the sodium bismuth titanate-based piezoelectric ceramic 33 Always in inverse relation to the depolarization temperature Td, i.e. increasing d 33 While always being accompanied by a decrease in Td and vice versa. Piezoelectric coefficient d of BNT-6BT piezoelectric ceramic 33 At 125pC/N, the depolarization temperature Td is about 100 ℃; piezoelectric coefficient d of ZnO doped BNT-6BT ceramic 33 80pC/N and a depolarization temperature Td of 150 ℃; BNT-6BT ceramic piezoelectric coefficient d after quenching treatment 33 145pC/N and a depolarization temperature Td of 136 ℃. At present, sodium bismuth titanate-based piezoelectric ceramics with excellent comprehensive performance can not be obtained, which hinders the application of the series of lead-free ceramics.
Thus, the preparation has a high piezoelectric coefficient d 33 And the sodium bismuth titanate lead-free piezoelectric ceramic material with high depolarization temperature Td has extremely important practical significance.
Disclosure of Invention
In order to solve the above technical problems, an object of the present invention is to provide a method for preparing a manganese-doped sodium bismuth titanate based lead-free piezoelectric ceramic, so that the prepared manganese-doped sodium bismuth titanate based lead-free piezoelectric ceramic has both high piezoelectric property and high temperature stability.
In order to achieve the technical purpose, the invention provides a preparation method of manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic, which comprises the following steps:
adding Bi 2 O 3 、Na 2 CO 3 、K 2 CO 3 、BaCO 3 、TiO 2 And MnO 2 Mixing, namely adding the mixture into absolute ethyl alcohol according to the mass ratio of 1 (1.2-1.5), ball-milling for 24-48 hours at the rotating speed of 200-;
adding absolute ethyl alcohol into the pre-sintered powder with the perovskite structure according to the formula 1 (1.2-1.5), ball-milling for 12-24 hours at the rotating speed of 200-230 r/min, drying at the temperature of 80-110 ℃, adding 7-8 w% of adhesive PVA, sieving by a 100-mesh sieve, and pressing for molding;
discharging the adhesive at 500-650 ℃ for 2-4 h, sintering at 1150-1200 ℃, and keeping the temperature for 2-3h, wherein the heating rate is 2-3 ℃/min, and the cooling rate is 4-5 ℃/min, so as to obtain the manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate ceramic wafer;
and plating gold on the sintered ceramic wafer for 10-20 min, and carrying out polarization treatment to obtain the manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic.
The preparation method of the invention is to use Bi 2 O 3 、Na 2 CO 3 、K 2 CO 3 、BaCO 3 、TiO 2 And MnO 2 Preparation of 0.79Bi as raw material 0.5 Na 0.5 TiO 3 -0.14Bi 0.5 K 0.5 TiO 3 -0.07BaTiO 3 The Mn ceramic sheet with x mol percent is finally plated with gold and polarized to obtain the manganese doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic.
In one embodiment of the present invention, the calcination temperature is 850-900 ℃, the calcination time is 2-3 hours, and the temperature rise rate is 5-6 ℃/min.
In a specific embodiment of the invention, the pressure forming is completed by keeping the pressure at 4MPa-8MPa for 2-3 min.
In one embodiment of the present invention, the polarization process comprises the steps of:
and (3) polarizing the ceramic wafer in an electric field of 50kV/cm-55kV/cm at 20-200 ℃ for 30-60 min.
The invention also provides manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramics, which is prepared by the preparation method.
In a specific embodiment of the invention, the structural formula of the manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic is 0.79Bi 0.5 Na 0.5 TiO 3 -0.14Bi 0.5 K 0.5 TiO 3 -0.07BaTiO 3 X mol% of Mn, wherein x is more than or equal to 0 and less than or equal to 1; preferably 0.1. ltoreq. x. ltoreq.0.25, within the range of the piezoelectric ceramicThe coefficient and the polarization temperature are higher.
In one embodiment of the present invention, the crystal structure of the manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic is a tetragonal phase and a pseudo-cubic phase coexisting at room temperature.
In one embodiment of the invention, the piezoelectric coefficient d of the manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic 33 150pC/N-180pC/N, depolarization temperature T d Is 165-185 ℃.
The manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic of the invention can be used for piezoelectric devices, including but not limited to filters, resonators and buzzers.
The manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate ceramic chip is put into a dielectric temperature spectrum tester, and dielectric properties of the ceramic chip are researched within the temperature range of 20-450 ℃, so that the depolarization temperature peak of the manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate ceramic is gradually reduced, and the ceramic chip is in the sharpest state when x is 0.25.
The manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic solves the problem that the high piezoelectric coefficient and the high depolarization temperature of the existing lead-free sodium bismuth titanate-based piezoelectric ceramic cannot be obtained at the same time, can induce a small amount of pseudo cubic phase to greatly improve the piezoelectric performance, and simultaneously keeps the high depolarization temperature, and has the chemical formula of 0.79Bi 0.5 Na 0.5 TiO 3 -0.14Bi 0.5 K 0.5 TiO 3 -0.07BaTiO 3 X mol% of Mn, wherein x is more than or equal to 0 and less than or equal to 1. The manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic has high piezoelectric property and high temperature stability, and can be used for piezoelectric devices such as filters, resonators and buzzers.
Drawings
FIG. 1 is an XRD spectrum of manganese doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic.
FIG. 2 is a surface SEM image of manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic.
FIG. 3 is a dielectric temperature spectrum of Mn-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic: wherein 1 denotes a frequency of 1kHz, 2 denotes a frequency of 10kHz, and 3 denotes a frequency of 100 kHz.
Detailed Description
The following detailed description of preferred embodiments of the invention will be made.
Example 1
This example provides a method for preparing piezoelectric ceramic, specifically to a method for preparing 0.79Bi by a sintering process of solid-phase reaction 0.5 Na 0.5 TiO 3 -0.14Bi 0.5 K 0.5 TiO 3 -0.07BaTiO 3 0.25 mol% Mn piezoelectric ceramic, comprising the following steps:
the method comprises the following steps:
weighing the raw material Bi according to the proportion of the chemical structural formula 2 O 3 、Na 2 CO 3 、K 2 CO 3 、BaCO 3 、TiO 2 And MnO 2 (that is, weighing each raw material according to the stoichiometric ratio of the structural formula), adding the prepared mixture (the specific dosage is not limited as long as the mixture is prepared according to the formula, in the embodiment, 100g of the mixture can be specifically prepared) into absolute ethyl alcohol according to the mass ratio of 1:1.3, then placing the mixture into a ball milling tank, ball milling the mixture for 24 hours by using a ball mill at the rotating speed of 230 revolutions/min, then drying the ball-milled mixture at 100 ℃, grinding the dried mixture by using a mortar to obtain mixed powder, placing the mixed powder into a corundum crucible, then placing the corundum crucible into a box furnace, and calcining the corundum crucible for 2 hours at 850 ℃ at the heating rate of 5 ℃/min to obtain the pre-sintered powder with the perovskite structure.
Step two:
and grinding the obtained pre-sintered powder in a mortar, putting the powder into a ball milling tank, adding absolute ethyl alcohol according to a ratio of 1:1.3, performing ball milling at 200 rpm for 24 hours, drying at 100 ℃, putting the powder into the mortar, grinding, adding 7 w% of adhesive PVA, sieving by a 100-mesh sieve, and maintaining the pressure at 6MPa for 3 minutes to press the powder into wafers with the diameter of 10 mm.
Step three:
and (3) stacking three formed wafers in a crucible paved with platinum sheets, discharging the adhesive at 550 ℃ for 3h, sintering at 1150 ℃, and preserving heat for 2h, wherein the heating rate is 2 ℃/min, the cooling rate is 4 ℃/min, so as to obtain 0.79Bi0.5Na0.5TiO3-0.14Bi0.5K0.5TiO3-0.07BaTiO3:0.25 mol% Mn ceramic wafers.
Step four:
and (3) plating gold on the sintered ceramic wafer for 10min by using a small-sized metal sputtering film plating machine, polarizing the ceramic wafer for 30min by using a direct-current high-voltage power supply at room temperature and a 50kV/cm electric field, and obtaining the 0.79Bi0.5Na0.5TiO3-0.14Bi0.5K0.5TiO3-0.07BaTiO3:0.25 mol% Mn piezoelectric ceramic (the process parameters in the steps only need to be within the range in the invention content, and the influence on the performance of a final product is small).
Performing structure and performance tests on the manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic
The method comprises the following steps: grinding and grinding the ceramic sample into powder for X-ray powder diffraction, wherein the specific test conditions are room temperature, the measurement angle range is 20-90 degrees, the adopted step length is 0.026 degrees, and the step length is 2 degrees per minute. According to the obtained X-ray powder diffraction spectrum, as shown in FIG. 1, it is shown that the manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate piezoelectric ceramic has a pure perovskite structure at room temperature, and a small amount of pseudo cubic phase appears in the Mn-doped ceramic.
Step two: after the obtained ceramic sample is subjected to gold spraying on the surface, the appearance of the ceramic surface is observed by using a scanning electron microscope, as shown in fig. 2, the size distribution of crystal grains in the ceramic chip is uniform, and the compactness is good.
Step three: and (3) performing dielectric temperature spectrum test on 0.79Bi0.5Na0.5TiO3-0.14Bi0.5K0.5TiO3-0.07BaTiO3:0.25 mol% Mn ceramic pieces obtained by polarization at room temperature, and then performing secondary polarization on the sample at the same polarization electric field and time at the depolarization temperature of 160 ℃ obtained by test to obtain the fully polarized ceramic sample. The dielectric constant and dielectric loss were measured at different temperatures at different test frequencies, and the depolarization temperature of the fully polarized ceramic was determined to be about 183 c, as shown in fig. 3.
Step four: using quasi-static d 33 The test system carries out in-situ d on the sample 33 Test, d 33 ＝180pC/N。
Example 2
This example provides a method for preparing 0.79Bi 0.5 Na 0.5 TiO 3 -0.14Bi 0.5 K 0.5 TiO 3 -0.07BaTiO 3 1 mol% Mn piezoelectric ceramic, which is substantially the same as example 1 except that: the content of Mn element is increased to 1 mol%; the piezoelectric coefficient d33 of the final product is 150pC/N, and the depolarization temperature Td is 165 ℃.
Example 3
This example provides a method for preparing 0.79Bi 0.5 Na 0.5 TiO 3 -0.14Bi 0.5 K 0.5 TiO 3 -0.07BaTiO 3 0.6 mol% Mn piezoelectric ceramic, which is substantially the same as in example 1 except that: the content of Mn element is increased to 1 mol%; the piezoelectric coefficient d33 of the final product is 160pC/N, and the depolarization temperature Td is 175 ℃.
Example 4
This example provides a method for preparing 0.79Bi 0.5 Na 0.5 TiO 3 -0.14Bi 0.5 K 0.5 TiO 3 -0.07BaTiO 3 0.10 mol% Mn piezoelectric ceramic, which is substantially the same as example 1 except that: the content of Mn element is only 0.10 mol%; the piezoelectric coefficient d33 of the final product is 170pC/N, and the depolarization temperature Td is 185 ℃.
The above embodiments are only for illustrating the technical idea and features of the present invention, and the purpose of the present invention is to enable those skilled in the art to understand the content of the present invention and implement the present invention, and not to limit the protection scope of the present invention by this means. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A preparation method of manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic is characterized by comprising the following steps:
adding Bi 2 O 3 、Na 2 CO 3 、K 2 CO 3 、BaCO 3 、TiO 2 And MnO 2 Mixing, adding the mixture according to the mass ratio of 1 (1.2-1.5)Ball-milling with water and ethanol at the rotation speed of 200-230 r/min for 24-48 hours, drying the ball-milled mixture at the temperature of 80-110 ℃, and calcining to obtain pre-sintered powder with a perovskite structure;
adding the pre-sintered powder with the perovskite structure into absolute ethyl alcohol according to the proportion of 1 (1.2-1.5), ball-milling for 12-24 hours at the rotating speed of 200-230 r/min, drying at the temperature of 80-110 ℃, adding 7-8 w% of adhesive PVA, sieving by a 100-mesh sieve, and pressing for molding;
discharging the adhesive at 500-650 ℃ for 2-4 h, sintering at 1150-1200 ℃, and keeping the temperature for 2-3h, wherein the heating rate is 2-3 ℃/min, and the cooling rate is 4-5 ℃/min, so as to obtain the manganese-doped sodium bismuth titanate-potassium bismuth titanate-barium titanate ceramic wafer;
and plating gold on the sintered ceramic wafer for 10-20 min, and carrying out polarization treatment to obtain the manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic.
2. The method for preparing the manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic as claimed in claim 1, wherein the calcination temperature is 850-900 ℃, the calcination time is 2-3 hours, and the temperature rise rate is 5-6 ℃/min.
3. The method for preparing the manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic according to claim 1, wherein the press forming is completed under the pressure of 4MPa-8MPa for 2-3 min.
4. The method for preparing manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic according to claim 1, wherein the polarization treatment comprises the following steps:
and (3) polarizing the ceramic wafer in an electric field of 50kV/cm-55kV/cm at 20-200 ℃ for 30-60 min.
5. The manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic is characterized in that: it is prepared by the preparation method of any one of claims 1 to 4.
6. The manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic according to claim 5, which isIs characterized in that: it has a chemical structural formula of 0.79Bi 0.5 Na 0.5 TiO 3 -0.14Bi 0.5 K 0.5 TiO 3 -0.07BaTiO 3 X mol% of Mn, wherein x is more than or equal to 0 and less than or equal to 1.
7. The manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic according to claim 6, wherein: its crystal structure is that at room temp. it is a mixture of tetragonal phase and pseudo-cubic phase.
8. The manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic according to claim 6, wherein: its piezoelectric coefficient d 33 150pC/N to 180pC/N, depolarization temperature T d Is 165-185 ℃.
9. The use of the manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic as claimed in claim 5, wherein: it is used for making piezoelectric device.
10. The use of the manganese-doped sodium bismuth titanate-based lead-free piezoelectric ceramic as claimed in claim 9, wherein: it is used in filters, resonators or buzzers.
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