CN111499377B - Piezoelectric ceramic and preparation method thereof - Google Patents

Piezoelectric ceramic and preparation method thereof Download PDF

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CN111499377B
CN111499377B CN202010404240.3A CN202010404240A CN111499377B CN 111499377 B CN111499377 B CN 111499377B CN 202010404240 A CN202010404240 A CN 202010404240A CN 111499377 B CN111499377 B CN 111499377B
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piezoelectric ceramic
ceramic
piezoelectric
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CN111499377A (en
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陈朗
马晓姿
袁国亮
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Southwest University of Science and Technology
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Abstract

The embodiment of the invention discloses piezoelectric ceramic and preparation thereofA method. The chemical general formula of the main component of the piezoelectric ceramic is as follows: (1-x) BiScO3‑xPbTiO3‑ySiO2Wherein x is more than or equal to 0.63 and less than or equal to 0.65, and y is more than or equal to 0.005 and less than or equal to 0.03. The preparation method of the piezoelectric ceramic is an oxide hot-pressing sintering method, and Bi is used2O3、Sc2O3、PbO、TiO2And SiO2The high-purity nano powder is used as a raw material, and the high-temperature piezoelectric ceramic with preferred orientation is obtained by utilizing a hot-pressing sintering process. The preparation method provided by the embodiment of the invention has the advantages of simple process, short preparation period and low production cost, and the prepared piezoelectric ceramic has the orientation degree of 87-98% and excellent piezoelectric performance. In addition, the preferentially oriented high-temperature piezoelectric ceramic provided by the embodiment of the invention also has good flexibility, and the minimum bending diameter of the preferentially oriented high-temperature piezoelectric ceramic can reach 2 mm after the preferentially oriented high-temperature piezoelectric ceramic is thinned into a thin sheet with the thickness of 8 microns, so that the preferentially oriented high-temperature piezoelectric ceramic can be used for high-temperature-resistant flexible electronic devices.

Description

Piezoelectric ceramic and preparation method thereof
Technical Field
The embodiment of the invention relates to a piezoelectric ceramic technology, in particular to a piezoelectric ceramic and a preparation method thereof.
Background
The piezoelectric ceramic material is used as an important branch of piezoelectric materials, and has excellent electrical and mechanical properties, so that the piezoelectric ceramic material has wide application in the fields of aerospace, radar, medical treatment and the like. Bismuth scandium titanate (BiScO)3-PbTiO3BS-PT) piezoelectric ceramic was first discovered in 2001, and the material exhibits a high piezoelectric constant and a curie temperature higher than 450 ℃, and is expected to be applied in the field of high-temperature electronic devices.
In order to further improve the piezoelectric property of the BS-PT ceramic, researchers carry out a great deal of research works such as substitution, doping, solid solution and the like on the BS-PT piezoelectric ceramic. At present, besides improving the piezoelectric performance of the ceramic by using methods such as substitution, doping, solid solution and the like, many researchers also optimize the structure and the piezoelectric performance of the piezoelectric ceramic by controlling the orientation of crystals, and the reaction template grain growth method is the most commonly used technology for preparing the oriented ceramic. However, the process for preparing the oriented ceramic by the reaction template grain growth method is complicated, the period is long, the preparation cost is high due to the high price of seed crystals, the thickness of a single-layer diaphragm is only dozens of microns due to the adoption of the tape casting process, the block ceramic is obtained in a laminating mode, the interlayer binding force is poor, the cracking is easy, and the deviation between the actual component and the preset component is easy to generate, so the reaction template crystalThe grain growth method is mainly used for laboratory research at present, and related products have poor cost performance and are difficult to carry out large-scale industrial application. In addition, some have adopted sol-gel method to prepare 0.36BiScO with preferred orientation3-0.64PbTiO3The (BS-PT) film prepared by the method has the advantages of obviously reduced piezoelectric constant compared with BS-PT high-temperature piezoelectric ceramics, complex process and higher preparation cost, and is not beneficial to the application of the BS-PT film in high-temperature piezoelectric electronic devices. Also, there have been methods of electrochemically inducing nucleation with BaCO3、TiO2And SiO2(Quartz) is used as raw material to prepare Ba with directional dendritic crystal structure2TiSi2O8-SiO2The method can obtain the ceramic material with higher orientation degree, but can generate deviation crystal due to the crushing of dendrite, and in addition, under the high-temperature environment, silicon dioxide can be reduced into monocrystalline silicon and then alloyed with platinum to generate corrosion phenomenon, so that the crystal orientation near the platinum wire is different.
In summary, the reaction template grain growth method is one of the most common methods for preparing oriented ceramics, and sol-gel is only suitable for the preparation of thin film materials, but both methods have the defects of complicated preparation process, long period, high cost and the like, which restrict the large-scale industrial production and application of the methods, while the electrochemical induced nucleation method for preparing oriented ceramics has a high threshold and is still in the laboratory research stage at present.
Disclosure of Invention
The embodiment of the invention provides piezoelectric ceramic and a preparation method thereof, and aims to prepare the piezoelectric ceramic with preferred orientation, good flexibility, high temperature resistance and excellent piezoelectric performance by simple process and low production cost.
To achieve the object, an embodiment of the present invention provides a piezoelectric ceramic and a method for preparing the same, wherein the piezoelectric ceramic comprises the following main components: (1-x) BiScO3-xPbTiO3-ySiO2Wherein x is more than or equal to 0.63 and less than or equal to 0.65, and y is more than or equal to 0.005 and less than or equal to 0.03.
Further, the preferred orientation of the piezoelectric ceramic is [100 ]]c、[110]cOr [111 ]]cOne of three pseudo cubic systems.
Furthermore, the raw material for preparing the piezoelectric ceramic comprises Bi2O3、Sc2O3、PbO、TiO2And SiO2High purity nano powder.
Further, the thickness of the piezoelectric ceramic is 7-9 micrometers, and the minimum bending diameter is 1.5-2.5 millimeters.
On one hand, the embodiment of the invention also provides piezoelectric ceramic and a preparation method thereof, wherein the method comprises the following steps:
bi in accordance with the stoichiometric ratio of the chemical formula of the main component of the piezoelectric ceramic2O3、Sc2O3、PbO、TiO2And SiO2Weighing the high-purity nano powder to obtain a raw material mixture of the piezoelectric ceramics;
performing ball milling, drying, calcining and grinding on the raw material mixture to obtain ceramic fine powder;
and carrying out hot-pressing sintering on the ceramic fine powder to obtain the piezoelectric ceramic.
Further, the step of performing ball milling, drying, calcining and grinding on the raw material mixture to obtain the ceramic fine powder comprises:
performing ball milling, drying and calcining on the raw material mixture to obtain ceramic powder;
and performing secondary ball milling, drying and grinding on the ceramic powder to obtain ceramic fine powder.
Further, after the raw material mixture is subjected to ball milling, drying and calcining to obtain ceramic powder, the method comprises the following steps:
and carrying out XRD diffraction test on the ceramic powder to judge whether the ceramic powder is pure phase or not.
Further, the time of ball milling and secondary ball milling is 8-12 hours, the ball milling speed is 200-.
Further, after the raw material mixture is subjected to ball milling, drying and calcining to obtain ceramic powder, the method comprises the following steps:
and carrying out XRD diffraction test on the ceramic powder to judge whether the ceramic powder is pure phase or not.
Furthermore, in the hot-pressing sintering process, the sintering temperature is 810-.
Further, the hot-pressing sintering of the ceramic fine powder to obtain the piezoelectric ceramic includes:
and thinning the piezoelectric ceramic to prepare the piezoelectric ceramic into a uniform sheet with the thickness of 7-9 mm and the minimum bending diameter of 1.5-2.5 mm.
Compared with the prior art, the embodiment of the invention at least has the following beneficial effects:
the chemical general formula of the main components of the piezoelectric ceramic is as follows: (1-x) BiScO3-xPbTiO3-ySiO2Wherein x is more than or equal to 0.63 and less than or equal to 0.65, y is more than or equal to 0.005 and less than or equal to 0.03, and the preferred orientation of the piezoelectric ceramic is [100 ]]c、[110]cOr [111 ]]cThe piezoelectric ceramic is one of three pseudo cubic crystal systems, can be thinned into a sheet with the thickness of 8 microns, has the minimum bending diameter of 2 millimeters, is easy to prepare, has better flexibility and high temperature resistance, and is suitable for most application scenes. SiO used in hot-pressing sintering adopted in the embodiment of the invention2The high-purity nano powder is used as a component of the raw material, can play a role in improving BS-PT base piezoelectric ceramics, effectively solves the problem of component deviation of a heterogeneous template in a reaction template grain growth method, and on the other hand, the SiO powder2The high-purity nano powder is combined with a hot pressing process, and plays a certain role in the preferential growth of BS-PT-based piezoelectric ceramic grains. In addition, the sintering temperature of the BS-PT base piezoelectric ceramic is reduced from more than 1000 ℃ to less than 900 ℃ in the sintering process, so that the damage of Pb volatilization to human bodies and the environment is effectively reduced. Compared with other ceramic preparation methods, the hot-pressing sintering adopted by the embodiment of the invention has the advantages of simple process, short preparation period, low production cost and the like.
Drawings
FIG. 1 is the present inventionPiezoelectric ceramic provided by the third embodiment of the invention is [100 ]]cPreferred orientation XRD test patterns;
FIG. 2 shows a piezoelectric ceramic composition [100 ] provided by the fourth embodiment of the present invention]cPreferred orientation XRD test patterns;
FIG. 3 shows a piezoelectric ceramic composition [100 ] according to the fifth embodiment of the present invention]cPreferred orientation XRD test patterns;
FIG. 4 shows a piezoelectric ceramic composition [100 ] according to a sixth embodiment of the present invention]cPreferred orientation XRD test patterns;
FIG. 5 shows a piezoelectric ceramic composition [110 ]]cPreferred orientation XRD test patterns;
FIG. 6 shows a piezoelectric ceramic composition [110 ]]cPreferred orientation XRD test patterns;
FIG. 7 shows a piezoelectric ceramic composition [110 ]]cPreferred orientation XRD test patterns;
FIG. 8 shows a piezoelectric ceramic composition [110 ]]cPreferred orientation XRD test patterns;
FIG. 9 shows a piezoelectric ceramic composition [111 ] according to an eleventh embodiment of the present invention]cPreferred orientation XRD test patterns;
FIG. 10 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 11 shows a piezoelectric ceramic composition [111 ] according to a thirteenth embodiment of the present invention]cPreferred orientation XRD test patterns;
FIG. 12 shows a piezoelectric ceramic composition [111 ] according to a fourteenth embodiment of the present invention]cPreferred orientation XRD test patterns;
FIG. 13 shows a piezoelectric ceramic composition [100 ] provided by fifteenth embodiment of the present invention]cPreferred orientation XRD test patterns;
FIG. 14 shows a piezoelectric ceramic element [100 ] according to a sixteenth embodiment of the present invention]cPreferred orientation XRD test patterns;
FIG. 15 shows a piezoelectric ceramic composition [100 ] according to a seventeenth embodiment of the present invention]cPreferred orientation XRD test pattern;
FIG. 16 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 17 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 18 shows a piezoelectric ceramic element [110 ] according to a twentieth embodiment of the present invention]cPreferred orientation XRD test patterns;
FIG. 19 shows a piezoelectric ceramic element [110 ] according to twenty-first embodiment of the present invention]cPreferred orientation XRD test patterns;
FIG. 20 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 21 shows a piezoelectric ceramic]cA preferred orientation XRD test pattern;
FIG. 22 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 23 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 24 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 25 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 26 shows a piezoelectric ceramic composition [100 ] provided in twenty-eight embodiments of the present invention]cA preferred orientation XRD test pattern;
FIG. 27 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 28 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 29 shows a piezoelectric ceramic element [110 ] provided in thirty-one embodiment of the invention]cPreferred orientation XRD test patterns;
FIG. 30 shows a thirty-two piezoelectric ceramic element [110 ]]cPreferred orientation XRD test patterns;
FIG. 31 shows a thirty-three piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 32 shows a thirty-four piezoelectric ceramic element [110 ]]cPreferred orientation XRD test patterns;
FIG. 33 shows a piezoelectric ceramic]cA preferred orientation XRD test pattern;
FIG. 34 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 35 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 36 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 37 shows a piezoelectric ceramic product [100 ] provided in thirty-nine embodiments of the present invention]cPreferred orientation XRD test patterns;
FIG. 38 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 39 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 40 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 41 is a schematic view of a forty-three piezoelectric ceramic piezoelectric element [110 ] according to example of the present invention]cPreferred orientation XRD test patterns;
FIG. 42 shows a forty-four piezoelectric ceramic]cA preferred orientation XRD test pattern;
FIG. 43 is a forty-five piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 44 is the present inventionPiezoelectric ceramic product [110 ] provided by forty-six inventive embodiments]cPreferred orientation XRD test patterns;
FIG. 45 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 46 shows a piezoelectric ceramic]cPreferred orientation XRD test patterns;
FIG. 47 shows a piezoelectric ceramic composition [111 ] in example forty-nine of the present invention]cPreferred orientation XRD test patterns;
FIG. 48 shows a piezoelectric ceramic]cPreferred orientation XRD test pattern.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples. It is to be understood that the specific embodiments described herein are for purposes of illustration and not limitation.
Example one
The embodiment of the invention provides piezoelectric ceramic and a preparation method thereof, wherein the main components of the piezoelectric ceramic have the chemical general formula: (1-x) BiScO3-xPbTiO3-ySiO2Wherein x is more than or equal to 0.63 and less than or equal to 0.65, and y is more than or equal to 0.005 and less than or equal to 0.03.
The specific preparation method of the piezoelectric ceramic in this embodiment is as follows:
(1) bi in accordance with the stoichiometric ratio of the chemical formula of the main component of the piezoelectric ceramic2O3、Sc2O3、PbO、TiO2And SiO2Weighing the high-purity nano powder to obtain a raw material mixture of the piezoelectric ceramics.
(2) And performing ball milling, drying, calcining and grinding on the raw material mixture to obtain ceramic fine powder.
(3) And carrying out hot-pressing sintering on the ceramic fine powder to obtain the piezoelectric ceramic.
In the embodiment, in the step (2), the raw material mixture is ball milled by wet milling with alcohol, specifically, the raw material mixture is placed in a polyethylene ball milling tank, and anhydrous ethanol accounting for 0.7-0.9 times of the total weight of the raw material mixture is added, in this embodiment, anhydrous ethanol accounting for 0.8 times of the total weight of the raw material mixture is added, and ball milled on a ball mill for 8-12 hours based on a ball milling speed of 200-300 rpm, in this embodiment, the ball milling speed is 250 rpm, and then the wet material of the raw material mixture after ball milling is poured into a petri dish and is moved to a drying oven at 60 ℃ for drying. Grinding the powder of the dried raw material mixture by using an agate mortar, then putting the ground powder into a clean corundum crucible, covering a corundum thin plate, putting the corundum thin plate into a muffle furnace, heating to 780-800 ℃ at the heating rate of 5 ℃/min, calcining for 2-4 hours, keeping the temperature for 2 hours, and cooling to room temperature along with the furnace to obtain the ceramic powder. Thereby completing the raw material pretreatment of the piezoelectric ceramic.
In this example, in step (3), after the pretreated raw material is obtained, hot press sintering of the ceramic fine powder is started to obtain the piezoelectric ceramic. Specifically, the ceramic fine powder is placed in a hot-pressing sintering mold, the upper surface and the lower surface of the pre-sintered ceramic fine powder are pressed for 30 minutes under the normal temperature by using the pressure of 8MPa to 12MPa, and then the pressure is reduced to 0MPa, so that a ceramic blank is obtained. Then heating the ceramic body from room temperature to 600 ℃ at the heating rate of 3 ℃/min, and then heating the ceramic body from 600 ℃ to the sintering temperature at the heating rate of 0.5-2 ℃/min, wherein the sintering temperature is 810 ℃ and 900 ℃. And when the temperature reaches the sintering temperature, increasing the pressure of the upper surface and the lower surface of the ceramic blank from 0MPa to 1-3MPa within 30 minutes, preserving the heat and the pressure for 7-10 hours, and then reducing the pressure to 0MPa within 60 minutes. And finally, reducing the temperature from the sintering temperature to 600 ℃ at the cooling rate of 0.5 ℃/minute, and then reducing the temperature of the ceramic from 600 ℃ to room temperature at the cooling rate of 1 ℃/minute to obtain the piezoelectric ceramic. The preferred orientation of the piezoelectric ceramic is [100 ]]c、[110]cOr [111 ]]cOne of three pseudo cubic systems.
According to the embodiment of the invention, the pressure is applied to the upper surface and the lower surface of the ceramic blank body along the vertical direction, so that the distance between solid particles along the direction of the applied pressure is reduced, and the solid-phase reaction is easier to occur. Meanwhile, the distance between the crystal grains in the direction vertical to the upper surface and the lower surface of the ceramic blank body is minimum, the energy required by crystal growth is minimum, the crystal is easier to preferentially grow along the low crystal face index direction, and finally the flexible high-temperature piezoelectric ceramic with preferred orientation is obtained.
Example two
The second embodiment of the invention provides a piezoelectric ceramic and a preparation method thereof, and the second embodiment of the invention is further explained on the basis of the first embodiment of the invention, wherein the general chemical formula of the main component of the piezoelectric ceramic is as follows: (1-x) BiScO3-xPbTiO3-ySiO2Wherein x is more than or equal to 0.63 and less than or equal to 0.65, and y is more than or equal to 0.005 and less than or equal to 0.03. Further, the preferred orientation of the piezoelectric ceramic is [100 ]]c、[110]cOr [111 ]]cOne of three pseudo cubic systems, the degree of orientation is 87% to 98%, and the relative density is 95% to 99%. Furthermore, the raw material for preparing the piezoelectric ceramic comprises Bi2O3、Sc2O3、PbO、TiO2And SiO2High purity nano powder. Further, the thickness of the piezoelectric ceramic is 8 μm, and the minimum bending diameter is 2 mm.
The specific preparation method of the piezoelectric ceramic in this embodiment is as follows:
(1) bi in accordance with the stoichiometric ratio of the chemical formula of the main component of the piezoelectric ceramic2O3、Sc2O3、PbO、TiO2And SiO2Weighing the high-purity nano powder to obtain a raw material mixture of the piezoelectric ceramics.
(2) And performing ball milling, drying and calcining on the raw material mixture to obtain ceramic powder.
(3) XRD diffraction test is carried out on the ceramic powder to judge whether the ceramic powder is pure phase or not.
(4) And performing secondary ball milling, drying and grinding on the ceramic powder to obtain ceramic fine powder.
(5) And carrying out hot-pressing sintering on the ceramic fine powder to obtain the piezoelectric ceramic.
(6) The piezoelectric ceramic is thinned to prepare the piezoelectric ceramic into a uniform thin sheet with the thickness of 7-9 mm and the minimum bending diameter of 1.5-2.5 mm.
In this embodiment, as preferable, step (3) is further added, an XRD diffraction test is performed on the ceramic powder to determine whether the ceramic powder is a pure phase, if so, the subsequent steps are performed, and if not, the steps (1) and (2) are adjusted according to actual conditions until the pure-phase ceramic powder is obtained.
In this embodiment, in the step (4), the ceramic powder is subjected to secondary ball milling for 8 to 12 hours on a ball mill based on a ball milling rate of 250 revolutions per minute, then a wet material of the ceramic powder subjected to the secondary ball milling is poured into a petri dish, and is moved to a 60-turn drying oven to be dried, and the dried ceramic powder is ground by an agate mortar to obtain uniform ceramic fine powder, thereby completing the raw material pretreatment of the piezoelectric ceramic.
In this embodiment, in step (6), the piezoelectric ceramic is further thinned to prepare the piezoelectric ceramic into a uniform sheet with a thickness of 7 to 9 mm, in this embodiment, the piezoelectric ceramic is thinned into a uniform sheet with a thickness of 8 mm, and then the uniform sheet is bent into an arc with a diameter of 1.5 to 2.5 mm and recovered by a manual bending manner, in this embodiment, the uniform sheet is bent into an arc with a diameter of 2 mm and recovered to obtain a uniform sheet with a thickness of 8 mm and a minimum bending diameter of 2 mm.
Further, after the preparation of the piezoelectric ceramic is completed, a performance characterization test may be performed on the piezoelectric ceramic to determine that the piezoelectric ceramic can be used, where the performance characterization test may include the following:
(1) the density of the high-temperature piezoelectric ceramic having a preferred orientation was measured by the archimedes drainage method, and the relative density of the ceramic was calculated.
(2) The degree of orientation of the ceramic, i.e. the degree of orientation f ═ P (P-P), can be obtained by calculation and analysis of the XRD pattern by the Lotgering method0)/(1-P0) Wherein P ═ I (I)(100)+I(200))/∑I(hkl)I is the relative intensity of the corresponding XRD diffraction peak, P0Is the P value of the free-oriented ceramic.
(3) After Ag electrodes are screen-printed on the upper and lower surfaces of the piezoelectric ceramic, the capacitance-temperature curve of the ceramic is measured by a dielectric temperature spectrometer and the Curie temperature T of the ceramic is confirmedc
(4) The above-mentioned alloy is charged with AgThe piezoelectric ceramic of the pole is soaked in silicone oil at 120 ℃, the electric field intensity is gradually increased from 0kV/cm to 50kV/cm by 5 times in a mode that the single amplitude is 10kV/cm, the piezoelectric ceramic is kept for 5 minutes under the corresponding electric field intensity after being increased for the first four times, the piezoelectric ceramic is polarized, and the piezoelectric ceramic is kept for 15 minutes when the electric field intensity is increased to 50kV/cm, and the piezoelectric ceramic is finally polarized. Then using quasi-static d33The measuring instrument measures the piezoelectric constant d of the piezoelectric ceramic subjected to the polarization process33
(5) Measuring the piezoelectric ceramic by an impedance analyzer to obtain the equivalent capacitance C and the equivalent resistance R of the ceramicnAnd calculating the tangent angle of dielectric loss (tan delta is 1/(omega CR)n) To express its dielectric loss.
(6) Measuring the piezoelectric ceramic by an impedance analyzer to obtain the planar resonance frequency (f) of the ceramicr1) And the plane anti-resonance frequency (f)a1) And calculating the plane electromechanical coupling coefficient
Figure GDA0003530881850000121
(7) The equivalent capacitance C of the flexible high-temperature piezoelectric ceramic with preferred orientation, the thickness t of the piezoelectric ceramic, the effective area A (overlapping area of upper and lower electrodes), and the vacuum dielectric constant (epsilon)0=8.85×10-12) Calculating the dielectric constant (. epsilon.) of the piezoelectric ceramicr=Ct/ε0A)。
(8) Repeating bending process 103And comparing the thinned thin sheet before and after bending by using a scanning electron microscope, and judging whether the ceramic thin sheet structure is damaged after multiple times of bending. Further, it is also possible to grow Ag electrodes on a ceramic sheet subjected to bending many times and to perform polarization. Soaking a ceramic sheet containing an Ag electrode in silicone oil at 120 ℃, gradually increasing the electric field strength from 0kV/cm to 50kV/cm in 5 times in a mode of single amplitude of 10kV/cm, keeping the electric field strength for 5 minutes after the electric field strength is increased for the first four times, polarizing the ceramic, keeping the electric field strength for 15 minutes when the electric field strength is increased to 50kV/cm, and finally polarizing the ceramic. The piezoelectric constant d of the ceramic sheet was then measured33. ThroughPiezoelectric constant d of multiply bent ceramic sheets33Compared with the attenuation of about 0.614% before multiple bending, the attenuation is low and can be ignored.
According to the embodiment of the invention, the obtained piezoelectric ceramic is thinned into a sheet with the thickness of 8 microns, the minimum bending diameter of the sheet is 2 millimeters, and the ceramic sheet has good flexibility; and, the ceramic sheet can be used for high temperature resistant flexible electronic devices because the Curie temperature of the ceramic is above 450 ℃.
EXAMPLE III
The third embodiment of the invention provides a piezoelectric ceramic and a preparation method thereof, and the third embodiment of the invention is further optimized on the basis of the second embodiment of the invention, and the chemical general formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.01SiO2That is, x is 0.635 and y is 0.01.
The specific preparation process of the third embodiment of the present invention is substantially the same as that of the second embodiment of the present invention, except that in the step (5) of this embodiment, the temperature of the ceramic body is raised from 600 ℃ to the sintering temperature of 810 ℃ at a temperature raising rate of 2 ℃/min, the pressure of the upper and lower surfaces of the ceramic body is increased from 0MPa to 1MPa, and the heat and pressure holding time is 7 hours.
The preferred orientation of the piezoelectric ceramic obtained in the third embodiment of the present invention is [100 ]]cDegree of orientation of 87% and piezoelectric constant d33876pC/N, piezoelectric constant d after bending33871pC/N, Curie temperature Tc452 deg.C, relative density 97%, dielectric loss tan delta 0.022, dielectric constant epsilonr1646, electromechanical coupling coefficient kp0.607. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD test pattern is shown in FIG. 1, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 13280a.u.
Example four
The fourth embodiment of the invention provides a piezoelectric ceramic and a preparation method thereof, and the fourth embodiment of the invention is further optimized on the basis of the second embodiment of the invention, and the chemical general formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.01SiO2I.e. x is 0.635,y=0.01。
The specific preparation process of the fourth embodiment of the present invention is substantially the same as that of the second embodiment of the present invention, except that in the step (5) of this embodiment, the temperature of the ceramic body is raised from 600 ℃ to the sintering temperature 815 ℃ at a temperature rise rate of 2 ℃/min, the pressure of the upper and lower surfaces of the ceramic body is increased from 0MPa to 3MPa, and the heat preservation and pressure maintaining time is 7 hours.
The preferred orientation of the piezoelectric ceramic obtained in the fourth embodiment of the present invention is [100 ]]cDegree of orientation of 90% and piezoelectric constant d33888pC/N, piezoelectric constant d after bending33882pC/N, Curie temperature Tc450 deg.C, relative density 98.5%, dielectric loss tan delta 0.024, and dielectric constant epsilonr1664, electromechanical coupling coefficient kp0.661. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD test pattern is shown in FIG. 2, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 12566a.u.
EXAMPLE five
The fifth embodiment of the invention provides a piezoelectric ceramic and a preparation method thereof, and the fifth embodiment of the invention is further optimized on the basis of the second embodiment of the invention, and the chemical general formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.01SiO2That is, x is 0.635 and y is 0.01.
The specific preparation process of the fifth embodiment of the present invention is substantially the same as that of the second embodiment of the present invention, except that in the step (5) of the present embodiment, the temperature of the ceramic body is increased from 600 ℃ to 825 ℃ at a temperature increase rate of 0.5 ℃/minute, the pressure of the upper and lower surfaces of the ceramic body is increased from 0MPa to 1MPa, and the heat and pressure holding time is 10 hours.
The preferred orientation of the piezoelectric ceramic obtained in the fifth embodiment of the present invention is [100 ]]cDegree of orientation of 94% and piezoelectric constant d33927pC/N, piezoelectric constant d after bending33925pC/N, Curie temperature Tc454 ℃, 97.9% relative density, 0.025% dielectric loss tan delta, and dielectric constant epsilonr1678, electromechanical coupling coefficient kp0.699. The piezoelectric ceramic is in [100 ]]cPreferred orientationThe XRD test pattern of (A) is shown in figure 3, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 17976a.u.
EXAMPLE six
The sixth embodiment of the invention provides piezoelectric ceramic and a preparation method thereof, and the sixth embodiment of the invention is further optimized on the basis of the second embodiment of the invention, and the chemical general formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.01SiO2That is, x is 0.635 and y is 0.01.
The specific preparation process of the sixth embodiment of the present invention is substantially the same as that of the second embodiment of the present invention, except that in the step (5) of this embodiment, the temperature of the ceramic body is raised from 600 ℃ to the sintering temperature of 830 ℃ at a temperature raising rate of 0.5 ℃/minute, the pressure of the upper and lower surfaces of the ceramic body is increased from 0MPa to 3MPa, and the heat and pressure holding time is 10 hours.
The preferred orientation of the piezoelectric ceramic obtained in the sixth embodiment of the present invention is [100 ]]cDegree of orientation of 89%, piezoelectric constant d33888pC/N, piezoelectric constant d after bending33881pC/N, Curie temperature Tc450 ℃, relative density of 99%, dielectric loss tan delta of 0.022, and dielectric constant epsilonr1658, electromechanical coupling coefficient kp0.641. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD pattern is shown in FIG. 4, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 11610a.u.
EXAMPLE seven
The seventh embodiment of the invention provides a piezoelectric ceramic and a preparation method thereof, and the seventh embodiment of the invention is further optimized on the basis of the second embodiment of the invention, and the chemical general formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.01SiO2That is, x is 0.635 and y is 0.01.
The specific preparation process of the seventh embodiment of the present invention is substantially the same as that of the second embodiment of the present invention, except that in the step (5) of this embodiment, the temperature of the ceramic body is raised from 600 ℃ to the sintering temperature of 845 ℃ at a temperature raising rate of 2 ℃/min, the pressure of the upper and lower surfaces of the ceramic body is increased from 0MPa to 1MPa, and the heat preservation and pressure maintaining time is 7 hours.
The preferred orientation of the piezoelectric ceramic obtained in the seventh embodiment of the present invention is [110 ]]cDegree of orientation of 88% and piezoelectric constant d33884pC/N, piezoelectric constant d after bending33876pC/N, Curie temperature Tc449 deg.C, relative density 96%, dielectric loss tan delta 0.022, and dielectric constant εr1662, electromechanical coupling coefficient kp0.618. The piezoelectric ceramic is in [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 5, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 17306a.u.
Example eight
The eighth embodiment of the invention provides piezoelectric ceramic and a preparation method thereof, and the eighth embodiment of the invention is further optimized on the basis of the second embodiment of the invention, and the chemical general formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.01SiO2That is, x is 0.635 and y is 0.01.
The specific preparation process of the eighth embodiment of the present invention is substantially the same as that of the second embodiment of the present invention, except that in the step (5) of this embodiment, the temperature of the ceramic body is raised from 600 ℃ to the sintering temperature of 850 ℃ at a temperature raising rate of 2 ℃/min, the pressure of the upper and lower surfaces of the ceramic body is increased from 0MPa to 3MPa, and the heat preservation and pressure maintaining time is 7 hours.
The preferred orientation of the piezoelectric ceramic obtained in the eighth embodiment of the present invention is [110 ]]cDegree of orientation of 92% and piezoelectric constant d33909pC/N, piezoelectric constant d after bending33903pC/N, Curie temperature Tc452 deg.C, relative density 96%, dielectric loss tan delta 0.021, and dielectric constant epsilonr1678, electromechanical coupling coefficient kp0.638. The piezoelectric ceramic is in [110 ]]cThe preferred orientation XRD pattern is shown in FIG. 6, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 20139a.u.
Example nine
Ninth embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and ninth embodiment of the present invention is further optimized based on the second embodiment of the present invention, and the piezoelectric ceramicThe chemical general formula of the main component of (A) is 0.365BiScO3-0.635PbTiO3-0.01SiO2That is, x is 0.635 and y is 0.01.
The specific preparation process of the ninth embodiment of the present invention is substantially the same as that of the second embodiment of the present invention, except that in the step (5) of this embodiment, the temperature of the ceramic body is raised from 600 ℃ to the sintering temperature of 860 ℃ at a temperature raising rate of 0.5 ℃/minute, the pressure of the upper and lower surfaces of the ceramic body is increased from 0MPa to 1MPa, and the heat and pressure holding time is 10 hours.
The preferred orientation of the piezoelectric ceramic obtained in the ninth embodiment of the present invention is [110 ]]cDegree of orientation of 96% and piezoelectric constant d33927pC/N, piezoelectric constant d after bending33921pC/N, Curie temperature Tc458 ℃, relative density of 97.3%, dielectric loss tan delta of 0.022, and dielectric constant epsilonr1689, electromechanical coupling coefficient kp0.651. The piezoelectric ceramic is in the area of [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 7, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 46374a.u.
Example ten
Tenth embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and tenth embodiment of the present invention is further optimized based on second embodiment of the present invention, and a chemical general formula of a main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.01SiO2That is, x is 0.635 and y is 0.01.
The specific preparation process of the tenth embodiment of the present invention is substantially the same as that of the second embodiment of the present invention, except that in the step (5) of this embodiment, the temperature of the ceramic body is increased from 600 ℃ to 865 ℃ at a temperature increase rate of 0.5 ℃/min, the pressure of the upper and lower surfaces of the ceramic body is increased from 0MPa to 3MPa, and the heat and pressure holding time is 10 hours.
The preferred orientation of the piezoelectric ceramic obtained in the embodiment of the present invention is [110 ]]cDegree of orientation of 89%, piezoelectric constant d33884pC/N, piezoelectric constant d after bending33881pC/N, Curie temperature Tc452 deg.C, relative density 98.7%, dielectric loss tan delta 0.023, dielectric constant epsilonr1672, electromechanical coupling coefficient kp0.614. The piezoelectric ceramic is in [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 8, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 29913a.u.
EXAMPLE eleven
The eleventh embodiment of the invention provides a piezoelectric ceramic and a preparation method thereof, and the eleventh embodiment of the invention is further optimized on the basis of the second embodiment of the invention, and the chemical general formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.01SiO2That is, x is 0.635 and y is 0.01.
The specific preparation process of the eleventh embodiment of the present invention is substantially the same as that of the second embodiment of the present invention, except that in the step (5) of this embodiment, the temperature of the ceramic body is raised from 600 ℃ to the sintering temperature 880 ℃ at a temperature raising rate of 2 ℃/min, the pressure of the upper and lower surfaces of the ceramic body is increased from 0MPa to 1MPa, and the heat and pressure holding time is 7 hours.
The preferred orientation of the piezoelectric ceramic obtained in the eleventh embodiment of the present invention is [111 ]]cDegree of orientation of 88% and piezoelectric constant d33960pC/N, piezoelectric constant d after bending33951pC/N, Curie temperature Tc453 ℃ C., relative density 98.1%, dielectric loss tan. delta. 0.021, and dielectric constant εr1668, electromechanical coupling coefficient kp0.623. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD pattern is shown in FIG. 9, which is at [111 ]]cThe diffraction intensity of the preferred orientation is 18837a.u.
Example twelve
Twelfth embodiment of the invention provides a piezoelectric ceramic and a preparation method thereof, and twelfth embodiment of the invention is further optimized on the basis of second embodiment of the invention, and the chemical general formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.01SiO2That is, x is 0.635 and y is 0.01.
The specific preparation process of the twelfth embodiment of the invention is basically the same as that of the second embodiment of the invention, except that in the step (5) of the embodiment, the temperature of the ceramic body is increased from 600 ℃ to the sintering temperature of 885 ℃ at the temperature increase rate of 2 ℃/min, the pressure of the upper surface and the lower surface of the ceramic body is increased from 0MPa to 3MPa, and the heat preservation and pressure maintaining time is 7 hours.
The preferred orientation of the piezoelectric ceramic obtained in the twelfth embodiment of the present invention is [111 ]]cDegree of orientation of 91% and piezoelectric constant d331002pC/N, piezoelectric constant d after bending33998pC/N, Curie temperature Tc450 ℃, relative density of 98.8%, dielectric loss tan delta of 0.022, and dielectric constant epsilonr1666, electromechanical coupling coefficient kp0.66. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD pattern is shown in FIG. 10, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 15030a.u.
EXAMPLE thirteen
Thirteenth embodiment of the present invention provides a piezoelectric ceramic and a method for manufacturing the same, and thirteenth embodiment of the present invention is further optimized based on second embodiment of the present invention, and the general chemical formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.01SiO2That is, x is 0.635 and y is 0.01.
The specific preparation process of the thirteenth embodiment of the present invention is substantially the same as that of the second embodiment of the present invention, except that in step (5) of this embodiment, the temperature of the ceramic body is raised from 600 ℃ to the sintering temperature of 895 ℃ at a temperature raising rate of 0.5 ℃/min, the pressure of the upper and lower surfaces of the ceramic body is increased from 0MPa to 1MPa, and the heat and pressure holding time is 10 hours.
The preferred orientation of the piezoelectric ceramic obtained in example thirteen of the present invention was [111 ]]cDegree of orientation of 95% and piezoelectric constant d331006pC/N, piezoelectric constant d after bending331002pC/N, curie temperature Tc453 ℃ C., relative density 98.8%, dielectric loss tan. delta. 0.025, and dielectric constant εr1686, electromechanical coupling coefficient kp0.669. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD pattern is shown in FIG. 11, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 39764a.u.
Example fourteen
Fourteenth embodiment of the present invention provides a piezoelectric ceramic and a method for manufacturing the same, wherein fourteenth embodiment of the present invention is further optimized based on the second embodiment of the present invention, and a chemical general formula of a main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.01SiO2That is, x is 0.635 and y is 0.01.
The specific preparation process of the fourteenth embodiment of the present invention is substantially the same as that of the second embodiment of the present invention, except that in step (5) of this embodiment, the temperature of the ceramic body is increased from 600 ℃ to 900 ℃ at a temperature increase rate of 0.5 ℃/min, the pressure of the upper and lower surfaces of the ceramic body is increased from 0MPa to 3MPa, and the heat-preserving and pressure-maintaining time is 10 hours.
The preferred orientation of the piezoelectric ceramic obtained in the fourteenth embodiment of the present invention is [111 ]]cDegree of orientation of 91% and piezoelectric constant d33923pC/N, piezoelectric constant d after bending33921pC/N, Curie temperature Tc448 ℃, relative density of 99.2%, dielectric loss tan delta of 0.022, and dielectric constant epsilonr1679, electromechanical coupling coefficient kp0.631. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD test pattern is shown in FIG. 12, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 27407a.u.
Example fifteen
Fifteenth in the embodiment of the present invention is a piezoelectric ceramic and a method for manufacturing the same, and fifteenth in the embodiment of the present invention is further optimized based on the third embodiment of the present invention, except that the general chemical formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of the fifteenth embodiment of the invention is the same as that of the fifteenth embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in the fifteenth embodiment of the invention is [100 ]]cDegree of orientation of 89%, piezoelectric constant d33860pC/N, piezoelectric constant d after bending33851pC/N, Curie temperature Tc439 ℃, relative density of 97%, dielectric loss tan delta of 0.024, dielectric constant epsilonr1660, electromechanical coupling coefficient kp0.623. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD pattern is shown in FIG. 13, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 15582a.u.
Example sixteen
Sixteenth embodiment of the present invention provides a piezoelectric ceramic and a method for manufacturing the same, where the sixteenth embodiment of the present invention is further optimized based on the fourth embodiment of the present invention, and the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of the sixteenth embodiment of the present invention is the same as that of the fourth embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in the sixteenth embodiment of the present invention is [100 ]]cDegree of orientation of 94% and piezoelectric constant d33845pC/N, piezoelectric constant d after bending33843pC/N, Curie temperature Tc438 deg.C, relative density 97.8%, dielectric loss tan delta 0.027, dielectric constant epsilonr1689, electromechanical coupling coefficient kp0.621. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD test pattern is shown in FIG. 14, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 16247a.u.
Example seventeen
Seventeenth embodiment of the present invention is further optimized based on the fifth embodiment of the present invention, and is different in that a chemical general formula of a main component of the piezoelectric ceramic is 0.365 bissco3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of the seventeenth embodiment of the invention is the same as that of the fifth embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in the seventeenth embodiment of the invention is [100 ]]cDegree of orientation of 93% and piezoelectric constant d33911pC/N, piezoelectric constant d after bending33906pC/N, Curie temperature Tc441 deg.C, relative density 97.7%, dielectric loss tan delta 0.026, and dielectric constant epsilonr1683, electromechanical couplingCoefficient kp0.661. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD pattern is shown in FIG. 15, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 62801a.u.
EXAMPLE eighteen
Eighteen embodiments of the present invention provide a piezoelectric ceramic and a method for manufacturing the same, and eighteen embodiments of the present invention are further optimized based on the sixth embodiment of the present invention, except that the general chemical formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of eighteen embodiments of the present invention is the same as that of sixteenth embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in eighteen embodiments of the present invention is [100 ]]cDegree of orientation of 88% and piezoelectric constant d33884pC/N, piezoelectric constant d after bending33876pC/N, Curie temperature Tc442 ℃, relative density of 98.2%, dielectric loss tan delta of 0.023, dielectric constant epsilonr1662, electromechanical coupling coefficient kp0.601. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD test pattern is shown in FIG. 16, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 49290a.u.
Example nineteen
Nineteenth embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and nineteenth embodiment of the present invention is further optimized on the basis of the seventh embodiment of the present invention, except that the chemical general formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of nineteenth embodiment of the present invention is the same as that of seventh embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in nineteenth embodiment of the present invention is [110 ]]cDegree of orientation of 88% and piezoelectric constant d33890pC/N, piezoelectric constant d after bending33881pC/N, Curie temperature Tc442 ℃, relative density 95.1%, dielectric loss tan delta 0.021, dielectric constant epsilonr1670, electromechanicalCoefficient of coupling kp0.626. The piezoelectric ceramic is in [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 17, which is at [110 ]]cThe diffraction intensity of the preferred orientation is 30644a.u.
Example twenty
Twenty embodiments of the present invention provide a piezoelectric ceramic and a method for manufacturing the same, and twenty embodiments of the present invention are further optimized based on the eighth embodiment of the present invention, except that a chemical general formula of a main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of the twenty embodiment of the present invention is the same as that of the eighth embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in the twenty embodiment of the present invention is [110 ]]cDegree of orientation of 90% and piezoelectric constant d33915pC/N, piezoelectric constant d after bending33910pC/N, Curie temperature Tc438 deg.C, relative density 95.9%, dielectric loss tan delta 0.023, dielectric constant epsilonr1677, electromechanical coupling coefficient kp0.660. The piezoelectric ceramic is in the area of [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 18, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 26505a.u.
Example twenty one
Twenty-first embodiment of the present invention provides a piezoelectric ceramic and a method for manufacturing the same, and twenty-first embodiment of the present invention is further optimized based on ninth embodiment of the present invention, except that a chemical general formula of a main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of twenty-first embodiment of the present invention is the same as that of ninth embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in twenty-first embodiment of the present invention is [110 ]]cDegree of orientation of 95% and piezoelectric constant d33929pC/N, piezoelectric constant d after bending33921pC/N, Curie temperature Tc439 ℃, relative density of 98.5%, dielectric loss tan delta of 0.025, and dielectric constant epsilonr1688, electromechanical coupling coefficient kp0.691. The piezoelectric ceramic is in the area of [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 19, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 67847a.u.
Example twenty two
Twenty-second embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and twenty-second embodiment of the present invention is further optimized based on tenth embodiment of the present invention, except that a chemical general formula of a main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of twenty-two in the embodiment of the present invention is the same as that in the embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in twenty-two in the embodiment of the present invention is [110 ]]cDegree of orientation of 92% and piezoelectric constant d33872pC/N, piezoelectric constant d after bending33866pC/N, Curie temperature Tc445 deg.C, relative density 97.7%, dielectric loss tan delta 0.024, and dielectric constant epsilonr1672, electromechanical coupling coefficient kp0.645. The piezoelectric ceramic is in the area of [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 20, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 56109a.u.
Example twenty three
Twenty-third embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and twenty-third embodiment of the present invention is further optimized based on the eleventh embodiment of the present invention, except that the chemical general formula of the main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of twenty-three in the embodiment of the invention is the same as that of the eleventh embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in twenty-three in the embodiment of the invention is [111 ]]cDegree of orientation of 88% and piezoelectric constant d33959pC/N piezoelectric constant d after bending33958pC/N, Curie temperature Tc441 deg.C, relative density of 98%, dielectricLoss tan delta 0.021, dielectric constant εr1656 electromechanical coupling coefficient kp0.642. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD pattern is shown in FIG. 21, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 15008a.u.
Example twenty-four
Twenty-fourth embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and twenty-fourth embodiment of the present invention is further optimized based on twelfth embodiment of the present invention, except that a chemical general formula of a main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of twenty-four in the embodiment of the present invention is the same as that of twelfth in the embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in twenty-four in the embodiment of the present invention is [111 ]]cDegree of orientation of 89%, piezoelectric constant d331021pC/N, piezoelectric constant d after bending331018pC/N, Curie temperature Tc442 ℃, relative density of 98.2%, dielectric loss tan delta of 0.021, and dielectric constant epsilonr1667, electromechanical coupling coefficient kp0.658. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD test pattern is shown in FIG. 22, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 17522a.u.
Example twenty-five
Twenty-fifth embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and twenty-fifth embodiment of the present invention is further optimized based on thirteenth embodiment of the present invention, except that a chemical general formula of a main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of twenty-five in the embodiment of the invention is the same as that of thirteen in the embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in twenty-five in the embodiment of the invention is [111 ]]cDegree of orientation of 93% and piezoelectric constant d331029pC/N, piezoelectric constant d after bending331021pC/N, Curie temperature Tc439 ℃, relative density of 97.9%, dielectric loss tan delta of 0.024, dielectric constant epsilonr1695, electromechanical coupling coefficient kp0.662. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD test pattern is shown in FIG. 23, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 14166a.u.
Example twenty-six
Twenty-sixth of the embodiments of the present invention provides a piezoelectric ceramic and a method for manufacturing the same, and twenty-sixth of the embodiments of the present invention is further optimized based on fourteenth of the embodiments of the present invention, except that a chemical general formula of a main component of the piezoelectric ceramic is 0.365BiScO3-0.635PbTiO3-0.03SiO2That is, x is 0.635 and y is 0.03.
The specific preparation process of twenty-six in the embodiment of the invention is the same as that of fourteen in the embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in twenty-six in the embodiment of the invention is [111 ]]cDegree of orientation of 92% and piezoelectric constant d33966pC/N, piezoelectric constant d after bending33959pC/N, Curie temperature Tc441 ℃, relative density of 97.5%, dielectric loss tan delta of 0.022, and dielectric constant epsilonr1692 electromechanical coupling coefficient kp0.625. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD test pattern is shown in FIG. 24, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 16884a.u.
Example twenty-seven
Twenty-seventh embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and twenty-seventh embodiment of the present invention is further optimized based on third embodiment of the present invention, except that a chemical general formula of a main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
The specific preparation process of twenty-seventh of the embodiment of the invention is the same as that of the embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained by twenty-seventh of the embodiment of the invention is [100 ]]cDegree of orientation of 87% and piezoelectric constant d33890pC/N, piezoelectric constant after bendingNumber d33882pC/N, Curie temperature Tc450 ℃, relative density 95.2%, dielectric loss tan delta 0.025, dielectric constant epsilonr1655, electromechanical coupling coefficient kp0.623. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD pattern is shown in FIG. 25, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 12434a.u.
Example twenty-eight
Twenty-eighth embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and twenty-eighth embodiment of the present invention is further optimized based on the fourth embodiment of the present invention, except that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
The specific preparation process of twenty-eight in the embodiment of the invention is the same as that of the fourth embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in twenty-eight in the embodiment of the invention is [100 ]]cDegree of orientation of 89%, piezoelectric constant d33873pC/N, piezoelectric constant d after bending33870pC/N, Curie temperature Tc448 ℃, relative density of 97.2%, dielectric loss tan delta of 0.021, and dielectric constant epsilonr1666, electromechanical coupling coefficient kp0.621. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD test pattern is shown in FIG. 26, which is at [100 ]]cThe diffraction intensity of the preferred orientation is 12600a.u.
Example twenty-nine
Twenty-ninth of the embodiments of the present invention is further optimized based on the fifth of the embodiments of the present invention, and the difference is that a chemical general formula of a main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
The specific preparation process of twenty-nine in the embodiment of the invention is the same as that of the fifth embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in twenty-nine in the embodiment of the invention is [100 ]]cDegree of orientation of 95% and piezoelectric constant d33926pC/N, piezoelectric constant d after bending33920pC/N, Curie temperature Tc448 ℃, relative density 95.8%, dielectric loss tan delta 0.023, dielectric constant epsilonr1692 electromechanical coupling coefficient kp0.663. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD test pattern is shown in FIG. 27, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 17989a.u.
Example thirty
Thirty embodiments of the invention provide a piezoelectric ceramic and a preparation method thereof, and thirty embodiments of the invention are further optimized on the basis of the sixth embodiment of the invention, and the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
The specific preparation process of thirty in the embodiment of the invention is the same as that of the sixth embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in the thirty embodiment of the invention is [100 ]]cDegree of orientation of 90% and piezoelectric constant d33876pC/N, piezoelectric constant d after bending33871pC/N, Curie temperature Tc450 ℃, relative density of 99%, dielectric loss tan delta of 0.021, and dielectric constant epsilonr1672, electromechanical coupling coefficient kp0.632. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD pattern is shown in FIG. 28, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 15148a.u.
Example thirty one
Thirty-first in the embodiments of the invention provides piezoelectric ceramic and a preparation method thereof, thirty-first in the embodiments of the invention is further optimized on the basis of the seventh in the embodiments of the invention, and the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
The specific preparation process of thirty-one in the embodiment of the invention is the same as that of the seventh embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in thirty-one in the embodiment of the invention is [110 ]]cThe degree of orientation is 89%Piezoelectric constant d33924pC/N, piezoelectric constant d after bending33920pC/N, Curie temperature Tc450 ℃, relative density of 97.3%, dielectric loss tan delta of 0.022, and dielectric constant epsilonr1665, electromechanical coupling coefficient kp0.672. The piezoelectric ceramic is in [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 29, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 24734a.u.
Example thirty-two
Thirty-two embodiments of the invention provide a piezoelectric ceramic and a preparation method thereof, and thirty-two embodiments of the invention are further optimized on the basis of the eighth embodiment of the invention, and the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
The specific preparation process of thirty-two in the embodiment of the invention is the same as that of the eighth in the embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained by thirty-two in the embodiment of the invention is [110 ]]cDegree of orientation of 91% and piezoelectric constant d33936pC/N, piezoelectric constant d after bending33932pC/N, Curie temperature Tc453 ℃ C., relative density 98.1%, dielectric loss tan δ 0.023, and dielectric constant εr1662, electromechanical coupling coefficient kp0.681. The piezoelectric ceramic is in the area of [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 30, which is at [110 ]]cThe diffraction intensity of the preferred orientation is 20186a.u.
Example thirty-three
Thirty-third embodiment of the invention provides piezoelectric ceramic and a preparation method thereof, thirty-third embodiment of the invention is further optimized on the basis of the ninth embodiment of the invention, and the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
The specific preparation process of thirty-three in the embodiment of the invention is the same as that of the ninth embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in thirty-three in the embodiment of the invention is[110]cDegree of orientation of 96% and piezoelectric constant d33954pC/N, piezoelectric constant d after bending33951pC/N, Curie temperature Tc452 deg.C, relative density 97.2%, dielectric loss tan delta 0.025, and dielectric constant epsilonr1695, electromechanical coupling coefficient kp0.685. The piezoelectric ceramic is in [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 31, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 30444a.u.
Example thirty-four
Thirty-fourth embodiment of the invention provides piezoelectric ceramic and a preparation method thereof, thirty-fourth embodiment of the invention is further optimized on the basis of tenth embodiment of the invention, and the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
The specific preparation process of thirty-four in the embodiment of the invention is the same as that of the embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in thirty-four in the embodiment of the invention is [110 ]]cDegree of orientation of 90% and piezoelectric constant d33903pC/N, piezoelectric constant d after bending33891pC/N, Curie temperature Tc459 deg.C, relative density 99%, dielectric loss tan delta 0.024, and dielectric constant epsilonr1687, electromechanical coupling coefficient kp0.641. The piezoelectric ceramic is in [110 ]]cThe preferred orientation XRD pattern is shown in FIG. 32, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 27273a.u.
Example thirty-five
Thirty-five embodiments of the invention provide a piezoelectric ceramic and a preparation method thereof, thirty-five embodiments of the invention are further optimized on the basis of the eleventh embodiment of the invention, and the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
The specific preparation process of thirty-five in the embodiment of the invention is the same as that of the eleventh embodiment of the invention, and thirty-five in the embodiment of the inventionFifthly, the preferred orientation of the obtained piezoelectric ceramic is [111 ]]cDegree of orientation of 90% and piezoelectric constant d33987pC/N, piezoelectric constant d after bending33984pC/N, curie temperature Tc452 deg.C, relative density 98.5%, dielectric loss tan delta 0.021, and dielectric constant epsilonr1672, electromechanical coupling coefficient kp0.631. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD pattern is shown in FIG. 33, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 9866a.u.
Example thirty-six
Thirty-six embodiments of the invention provide a piezoelectric ceramic and a preparation method thereof, thirty-six embodiments of the invention are further optimized on the basis of twelve embodiments of the invention, and the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
The specific preparation process of thirty-six in the embodiment of the invention is the same as that of the twelfth embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in thirty-six in the embodiment of the invention is [111 ]]cDegree of orientation of 94% and piezoelectric constant d331005pC/N, piezoelectric constant d after bending33998pC/N, Curie temperature Tc450 ℃, relative density of 98.3%, dielectric loss tan delta of 0.024, and dielectric constant epsilonr1660, electromechanical coupling coefficient kp0.662. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD test pattern is shown in FIG. 34, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 11811a.u.
Example thirty-seven
Thirty-seventh embodiment of the invention provides piezoelectric ceramic and a preparation method thereof, thirty-seventh embodiment of the invention is further optimized on the basis of thirteen embodiment of the invention, and the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
Thirty-seven specific preparation process of embodiment of the invention and the inventionIn the same manner as in thirteen example, the preferred orientation of the piezoelectric ceramic obtained in thirty-seven examples of the present invention is [111 ]]cDegree of orientation of 96% and piezoelectric constant d331010pC/N, piezoelectric constant d after bending331009pC/N, Curie temperature Tc451 ℃, 97.2% relative density, 0.025% dielectric loss tan delta, and dielectric constant epsilonr1672, electromechanical coupling coefficient kp0.691. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD pattern is shown in FIG. 35, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 32002a.u.
Example thirty-eight
Thirty-eight embodiment of the invention provides piezoelectric ceramic and a preparation method thereof, thirty-eight embodiment of the invention is further optimized on the basis of fourteen embodiment of the invention, and the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.01SiO2That is, x is 0.645 and y is 0.01.
The specific preparation process of thirty-eight in the embodiment of the invention is the same as that of fourteen in the embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in thirty-eight in the embodiment of the invention is [111 ]]cDegree of orientation of 90% and piezoelectric constant d33944pC/N, piezoelectric constant d after bending33942 pC/N, Curie temperature Tc448 ℃, relative density of 98.3%, dielectric loss tan delta of 0.024, dielectric constant epsilonr1675, electromechanical coupling coefficient kp0.632. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD test pattern is shown in FIG. 36, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 28337a.u.
Example thirty-nine
Thirty-ninth embodiment of the invention provides piezoelectric ceramic and a preparation method thereof, and thirty-ninth embodiment of the invention is further optimized on the basis of the third embodiment of the invention, and is different in that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03.
Practice of the inventionThe specific preparation process of thirty-nine example is the same as that of the embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in thirty-nine example of the present invention is [100 ]]cDegree of orientation of 90% and piezoelectric constant d33877pC/N, piezoelectric constant d after bending33869pC/N, Curie temperature Tc441 ℃, relative density of 95%, dielectric loss tan delta of 0.021, and dielectric constant epsilonr1670, electromechanical coupling coefficient kp0.611. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD pattern is shown in FIG. 37, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 17925a.u.
Example forty
Embodiment forty of the present invention provides a piezoelectric ceramic and a preparation method thereof, and embodiment forty of the present invention is further optimized on the basis of embodiment forty of the present invention, but the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03.
The specific preparation process of example forty of the present invention is the same as that of example forty of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in example forty of the present invention is [ 100%]cDegree of orientation of 92% and piezoelectric constant d33914pC/N, piezoelectric constant d after bending33910pC/N, Curie temperature Tc442 ℃ C., relative density 95.3%, dielectric loss tan. delta. 0.022, and dielectric constant εr1685, electromechanical coupling coefficient kp0.634. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD test pattern is shown in FIG. 38, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 14148a.u.
Example forty one
Forty first embodiment of the present invention provides a piezoelectric ceramic and a preparation method thereof, and forty first embodiment of the present invention is further optimized on the basis of the fifth embodiment of the present invention, but the difference is that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03.
The specific preparation process of forty-one embodiment of the present invention is the same as that of the fifth embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in forty-one embodiment of the present invention is [100 ]]cDegree of orientation of 98% and piezoelectric constant d33950pC/N, piezoelectric constant d after bending33947pC/N, Curie temperature Tc439 ℃, relative density of 98%, dielectric loss tan delta of 0.025, dielectric constant epsilonr1692 electromechanical coupling coefficient kp0.668. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD test pattern is shown in FIG. 39, which is at [100 ]]cThe diffraction intensity of the preferred orientation was 20941a.u.
Example forty two
Forty-second embodiment of the present invention provides a piezoelectric ceramic and a preparation method thereof, and forty-second embodiment of the present invention is further optimized based on the sixth embodiment of the present invention, and is different in that a chemical general formula of a main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03.
The specific preparation process of forty two in the embodiment of the present invention is the same as that of the sixth embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in forty two in the embodiment of the present invention is [100 ]]cDegree of orientation of 90% and piezoelectric constant d33888pC/N, piezoelectric constant d after bending33883pC/N, Curie temperature Tc438 deg.C, relative density 98%, dielectric loss tan delta 0.023, dielectric constant epsilonr1666, electromechanical coupling coefficient kp0.623. The piezoelectric ceramic is in [100 ]]cThe preferred orientation XRD pattern is shown in FIG. 40, which is at [100 ]]cThe diffraction intensity of the preferred orientation is 22922a.u.
Example forty-three
Forty-third embodiment of the invention provides piezoelectric ceramic and a preparation method thereof, and forty-third embodiment of the invention is further optimized on the basis of the seventh embodiment of the invention, and is different in that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03。
The specific preparation process of forty-three in the embodiment of the invention is the same as that of the seventh embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in forty-three in the embodiment of the invention is [110 ]]cDegree of orientation of 89%, piezoelectric constant d33881pC/N, piezoelectric constant after bending d33874pC/N, Curie temperature Tc440 ℃, relative density of 97.5%, dielectric loss tan delta of 0.022, and dielectric constant epsilonr1623, electromechanical coupling coefficient kp0.636. The piezoelectric ceramic is in [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 41, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 18130a.u.
Example forty-four
Forty-fourth embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and forty-fourth embodiment of the present invention is further optimized based on eighth embodiment of the present invention, but is different in that a chemical general formula of a main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03.
The specific preparation process of forty-four in the embodiment of the present invention is the same as that of the eighth embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in forty-four in the embodiment of the present invention is [110 ]]cDegree of orientation of 93% and piezoelectric constant d33890pC/N, piezoelectric constant d after bending33883pC/N, Curie temperature Tc441 ℃, relative density of 97.7%, dielectric loss tan delta of 0.024, and dielectric constant epsilonr1675, electromechanical coupling coefficient kp0.657. The piezoelectric ceramic is in [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 42, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 22618a.u.
Example forty-five
Forty-five embodiments of the present invention provide a piezoelectric ceramic and a method for producing the same, and forty-five embodiments of the present invention are further optimized based on the ninth embodiment of the present invention, but the difference is that a chemical general formula of a main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03.
The specific preparation process of forty-five in the embodiment of the invention is the same as that of the ninth embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in the forty-five in the embodiment of the invention is [110 ]]cDegree of orientation 97%, piezoelectric constant d33927pC/N, piezoelectric constant d after bending33921pC/N, Curie temperature Tc444 ℃, relative density of 98%, dielectric loss tan delta of 0.025, and dielectric constant epsilonr1685, electromechanical coupling coefficient kp0.664. The piezoelectric ceramic is in [110 ]]cThe preferred orientation XRD pattern is shown in FIG. 43, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 104329a.u.
Example forty-six
Forty-six embodiments of the present invention provide a piezoelectric ceramic and a method for producing the same, and forty-six embodiments of the present invention are further optimized based on the tenth embodiment of the present invention, but the difference is that a chemical general formula of a main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03.
The specific preparation process of forty-six in the embodiment of the present invention is the same as that in the embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in forty-six in the embodiment of the present invention is [110 ]]cDegree of orientation of 90% and piezoelectric constant d33902pC/N, piezoelectric constant d after bending33900pC/N, Curie temperature Tc441 ℃, relative density of 98.9%, dielectric loss tan delta of 0.024, and dielectric constant epsilonr1662, electromechanical coupling coefficient kp0.629. The piezoelectric ceramic is in the area of [110 ]]cThe preferred orientation XRD test pattern is shown in FIG. 44, which is at [110 ]]cThe diffraction intensity of the preferred orientation was 74733a.u.
Example forty-seven
Forty-seventh embodiment of the invention provides piezoelectric ceramic and a preparation method thereof, and forty-seventh embodiment of the invention is further optimized on the basis of eleventh embodiment of the invention, and is different in that the chemical general formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03.
The specific preparation process of forty-seven in the embodiment of the invention is the same as that of the eleventh in the embodiment of the invention, and the preferred orientation of the piezoelectric ceramic obtained in forty-seven in the embodiment of the invention is [111 ]]cDegree of orientation of 89%, piezoelectric constant d33984pC/N, piezoelectric constant d after bending33979pC/N, Curie temperature Tc439 ℃, relative density of 97%, dielectric loss tan delta of 0.022, and dielectric constant epsilonr1660, electromechanical coupling coefficient kp0.659. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD pattern is shown in FIG. 45, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 9866a.u.
Example forty-eight
Forty-eight embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and forty-eight embodiment of the present invention is further optimized based on the twelfth embodiment of the present invention, and is different in that a chemical general formula of a main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03.
The specific preparation process of forty-eight in the embodiment of the present invention is the same as that of the twelfth embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in forty-eight in the embodiment of the present invention is [111 ]]c93% of degree of orientation and piezoelectric constant d33978pC/N, piezoelectric constant d after bending33974pC/N, Curie temperature Tc439 ℃, relative density of 98.2%, dielectric loss tan delta of 0.023, dielectric constant epsilonr1669, electromechanical coupling coefficient kp0.642. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD test pattern is shown in FIG. 46, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 11783a.u.
Example forty-nine
Forty-ninth embodiment of the present invention provides a piezoelectric ceramic and a method for producing the same, and forty-ninth embodiment of the present invention is further optimized on the basis of thirteen embodiment of the present invention, except that the piezoelectric ceramic is one of piezoelectric ceramics and piezoelectric ceramics, and the method for producing the sameThe chemical formula of the main component of the ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03.
The specific preparation process of forty-nine in the embodiment of the present invention is the same as that of the thirteenth embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in forty-nine in the embodiment of the present invention is [111 ]]cDegree of orientation 97% and piezoelectric constant d33978pC/N, piezoelectric constant d after bending33974pC/N, Curie temperature Tc439 ℃, relative density of 98.2%, dielectric loss tan delta of 0.023, dielectric constant epsilonr1669, electromechanical coupling coefficient kp0.642. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD pattern is shown in FIG. 47, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 67573a.u.
Example fifty
Fifty embodiments of the present invention provide a piezoelectric ceramic and a method for preparing the same, fifty embodiments of the present invention are further optimized based on fourteen embodiments of the present invention, and the difference is that the general chemical formula of the main component of the piezoelectric ceramic is 0.355BiScO3-0.645PbTiO3-0.03SiO2That is, x is 0.645 and y is 0.03.
The specific preparation process of fifty in the embodiment of the present invention is the same as that of fourteen in the embodiment of the present invention, and the preferred orientation of the piezoelectric ceramic obtained in fifty in the embodiment of the present invention is [111 ]]cDegree of orientation of 89%, piezoelectric constant d33977pC/N, piezoelectric constant d after bending33971pC/N, Curie temperature Tc441 ℃, relative density of 97.8%, dielectric loss tan delta of 0.021, and dielectric constant epsilonr1665, electromechanical coupling coefficient kp0.638. The piezoelectric ceramic is in [111 ]]cThe preferred orientation XRD test pattern is shown in FIG. 48, which is at [111 ]]cThe diffraction intensity of the preferred orientation was 61768a.u.
It is to be noted that the foregoing is only illustrative of the preferred embodiments of the present invention and the technical principles employed. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, although the present invention has been described in greater detail by the above embodiments, the present invention is not limited to the above embodiments, and may include other equivalent embodiments without departing from the spirit of the present invention, and the scope of the present invention is determined by the scope of the appended claims.

Claims (7)

1. A piezoelectric ceramic, characterized in that the chemical formula of the main component of the piezoelectric ceramic is: (1-x) BiScO3-xPbTiO3-ySiO2Wherein x is more than or equal to 0.63 and less than or equal to 0.65, and y is more than or equal to 0.005 and less than or equal to 0.03;
the preferred orientation of the piezoelectric ceramic is [100 ]]c、[110]cOr [111 ]]cOne of three pseudo cubic systems;
bi in accordance with the stoichiometric ratio of the chemical formula of the main component of the piezoelectric ceramic2O3、Sc2O3、PbO、TiO2And SiO2Weighing the high-purity nano powder to obtain a raw material mixture of the piezoelectric ceramics;
performing ball milling, drying, calcining and grinding on the raw material mixture to obtain ceramic fine powder;
and carrying out hot-pressing sintering on the ceramic fine powder to obtain the piezoelectric ceramic.
2. The piezoelectric ceramic according to claim 1, wherein the piezoelectric ceramic has a thickness of 7 to 9 μm and a minimum bending diameter of 1.5 to 2.5 mm.
3. The piezoelectric ceramic according to claim 1, wherein the ball-milling, drying, calcining and grinding the raw material mixture to obtain the ceramic fine powder comprises:
performing ball milling, drying and calcining on the raw material mixture to obtain ceramic powder;
and performing secondary ball milling, drying and grinding on the ceramic powder to obtain ceramic fine powder.
4. The piezoelectric ceramic of claim 3, wherein the time for ball milling and secondary ball milling is 8-12 hours, the ball milling rate is 200-300 rpm, the ball milling medium for ball milling and secondary ball milling is absolute ethyl alcohol, and the weight of the ball milling medium is 0.7-0.9 times of the weight of the raw material mixture.
5. The piezoelectric ceramic according to claim 3, wherein the ceramic powder obtained by ball-milling, drying and calcining the raw material mixture comprises:
and carrying out XRD diffraction test on the ceramic powder to judge whether the ceramic powder is pure phase or not.
6. The piezoelectric ceramic according to claim 1, wherein in the hot pressing sintering process, the sintering temperature is 810-900 ℃, the hot pressing pressure is 1-3MPa, the heating rate to the sintering temperature is 0.5-2 ℃/min, and the heat preservation and pressure maintaining time is 7-10 hours.
7. The piezoelectric ceramic according to claim 1, wherein the hot press sintering of the ceramic fine powder to obtain the piezoelectric ceramic comprises:
and thinning the piezoelectric ceramic to prepare the piezoelectric ceramic into a uniform sheet with the thickness of 7-9 micrometers and the minimum bending diameter of 1.5-2.5 millimeters.
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