CN113880575A - Doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material and preparation method thereof - Google Patents

Doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material and preparation method thereof Download PDF

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CN113880575A
CN113880575A CN202111356811.1A CN202111356811A CN113880575A CN 113880575 A CN113880575 A CN 113880575A CN 202111356811 A CN202111356811 A CN 202111356811A CN 113880575 A CN113880575 A CN 113880575A
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piezoelectric ceramic
temperature
zirconate titanate
powder
lead
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CN113880575B (en
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余方云
张秀琴
刘如峰
邱俊
宋有望
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Jiangsu Wave Speed Sensor Co ltd
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Jiangsu Wave Speed Sensor Co ltd
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Abstract

The invention discloses a doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material and a preparation method thereof, wherein the piezoelectric ceramic comprises xPb (Mn)1/3Nb2/3)]O3‑(1‑x)Pb(Zr0.52Ti0.48)]O3‑ywt％Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3‑zwt％La0.1Bi0.9FeO3Wherein the value range of x is 0.04-0.06, the value range of y is 0.5-3, and the value range of z is 0.1-0.3. In the preparation process, a high-temperature solid-phase synthesis method is adopted, and the sintering temperature in the synthesis process is effectively improved by controlling the range of y and z parametersThe relative dielectric constant, the d33 constant and the Curie temperature of the prepared piezoelectric ceramic material are improved, the temperature sensitivity and the application range of the material are improved, the preparation process is simple, raw materials are easy to obtain, and the technical problems that the existing material is not favorable for being used in a high-temperature and high-pressure environment due to insufficient Curie temperature and the sensitivity of a sensor caused by insufficient d33 constant can be limited are solved.

Description

Doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material and preparation method thereof
Technical Field
The invention relates to a piezoelectric ceramic material, in particular to a doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material and a preparation method thereof.
Background
The piezoelectric material is an important functional material for realizing the interconversion of mechanical energy and electric energy, has wide application in various electronic components such as sensors, ultrasonic transducers, resonators, buzzers, electronic ignition and the like, has the advantages of simple preparation process, low manufacturing cost, excellent piezoelectric performance, adjustable components and the like, and is one of the research and development hotspots in the field of materials. In the fields of energy, aviation, aerospace, automobiles, petrochemical engineering, geological exploration and the like, a high-precision driver and a high-precision sensor are required to work in a high-temperature harsh environment, and the sensitivity of a piezoelectric device in a high-temperature environment and a low-temperature environment is extremely high.
The current commercial high-temperature sensor material is mainly LiNbO3The isobaric pressure single crystal material has the disadvantages of high cost, poor single crystal performance, insufficient Curie temperature and no contribution to the use in high-temperature and high-pressure environments; in addition, with the increasing application of miniaturized devices, the demands for high functionality and miniaturization of piezoelectric ceramics are increasing. Generally, when the piezoelectric coefficient d33 of the ceramic is not large, the sensitivity of the whole sensor is limited, and generally, in order to increase the charge sensitivity of the sensor, an important approach is to increase the weight of the mass block, which may result in an increase in the volume and weight of the sensor, and a decrease in the operating frequency, which is not favorable for the application of the sensor in the conditions of high temperature of the operating environment and insufficient space, and is also difficult to adapt to the field with high sensitivity requirement.
Disclosure of Invention
The invention provides a doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material and a preparation method thereof, aiming at solving the technical problems of insufficient sensitivity, low Curie temperature and overlarge volume of the piezoelectric ceramic in the field of the piezoelectric ceramic at present.
The technical scheme of the invention is as follows: provides a doped lead manganese niobate-a piezoelectric ceramic material of lead zirconate titanate with the stoichiometric formula xPb (Mn)1/3Nb2/3)]O3-(1-x)Pb(Zr0.52Ti0.48)]O3-ywt％Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3-zwt％La0.1Bi0.9FeO3Wherein the value range of x is 0.04-0.06, the value range of y is 0.5-3, and the value range of z is 0.1-0.3.
In order to realize the technical scheme, the invention also provides a preparation method of the doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material, which comprises the following steps:
s1: preparation of Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3Pre-sintered powder
According to the formula Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3Weighing analytically pure BaCO3、SrCO3、SnO2、Mg2(OH)2CO3、TiO2、ZrO2Powder, performing first ball milling on the raw materials under the condition of taking ethanol as a dispersing agent, and drying to obtain a precursor of the reaction; then putting the mixed powder into an alumina crucible for pre-sintering, and then carrying out secondary ball milling to obtain Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3Pre-burning the powder;
s2: preparation of La0.1Bi0.9FeO3Pre-sintered powder
According to the formula La0.1Bi0.9FeO3Weighing analytically pure Bi2O3、Fe2O3Mixing the raw materials under the condition of a dispersing agent, performing primary ball milling, and drying to obtain a precursor of the reaction; then placing the mixed powder into an alumina crucible for presintering, and then carrying out ball milling and crushing to obtain La0.1Bi0.9FeO3Pre-burning the powder;
s3: ingredients
Raw materials are mixed according to a composition formula
xPb(Mn1/3Nb2/3)]O3-(1-x)Pb(Zr0.52Ti0.48)]O3-ywt％Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3-zwt％La0.1Bi0.9FeO3Weighing Pb3O4、MnO2、Nb2O5、ZrO2、TiO2Mixing materials, wherein the value range of x is 0.04-0.06, the value range of y is 0.5-3, the value range of z is 0.1-0.3, and Ba accounting for 0.5-3 wt% of the mass ratio of the main components is weighed0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3And 0.1 to 0.3 weight percent of La0.1Bi0.9FeO3. In which Pb is3O4The Ba is chemically pure, and other raw materials are analytically pure0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3And La0.1Bi0.9FeO3Mixing the raw materials in a ball milling tank, and drying the raw materials to obtain a mixture, wherein the mixture is obtained by synthesizing the S1 and the S2;
s4: synthesis of
Putting the dried powder of S3 into an alumina crucible, compacting and compacting, and performing high-temperature solid phase synthesis after capping and sealing;
s5: water milling and drying
Ball-milling and drying the synthetic material of S4 again;
s6: fine grinding
Finely grinding the dried powder of S5 to ensure that the particle size D50 is 0.3-0.6 um;
s7: shaping and plastic discharge
Molding the powder prepared in the step S6 to prepare a blank, and then performing plastic removal treatment;
s8: sintering
And (4) burying and burning the blank body of the organic matters discharged in the step (S7) by adopting lead zirconate titanate powder, and then cooling along with the furnace to obtain the piezoelectric ceramic piece.
Further, the first ball milling time in S1 is 6-8h, and the pre-sintering temperature is 950-1050 ℃; the pre-sintering time is 2 hours, and the second ball milling time is 6 hours.
Further, in S2, the pre-firing temperature is 900 ℃, the pre-firing time is 2 hours, and the ball milling time is 6 hours.
Further, when the materials are mixed in the ball milling tank in S3, the ratio of the balls: material preparation: the weight ratio of water is 2:1:0.5, and the ball milling time is 6-8 h.
Further, the temperature of high-temperature solid-phase synthesis in S4 is 950-1050 ℃, and the reaction time is 2 h.
Further, the molding and plastic-discharging process in S7 includes: adding 14-16 wt% of polyvinyl butyral, an organic solvent, a dispersing agent and a leveling agent into the fine ground powder obtained in the step S6 to prepare slurry for tape casting, and punching into a wafer; granulating the obtained wafer, pressing into large blocks, aging the large blocks of blanks for 48h, grinding and granulating, and sieving the particles with a 100-mesh sieve; molding the obtained sieve material under the pressure of 8-10 MPa by using a mold with the diameter of 10mm to obtain a blank with certain strength and the thickness of 2.1 mm; then heating the blank body to 200 ℃ at the speed of 3 ℃/min, then heating the blank body from 200 ℃ to 400 ℃ at the speed of 1.5 ℃/min, preserving the heat at 400 ℃ for 30min, then heating the blank body to 550 ℃ at the speed of 5 ℃/min, preserving the heat for 10min, and discharging organic matters.
Further, the burying sintering in the S8 is carried out in a box type furnace, the heating rate is 3 ℃/min, the final temperature is 1200-1250 ℃, and the heat preservation time is 70 min.
Further, the method comprises the testing step of:
s9: silver firing
Carrying out silver firing treatment on the sintered piezoelectric ceramic sheet in the S8;
s10: polarization of
Polarizing the silver-fired product of S9 under specified conditions;
s11: testing piezoelectric performance
Standing the piezoelectric ceramic sheet subjected to S10 polarization treatment at room temperature for 24h, testing the piezoelectric performance of the piezoelectric ceramic sheet, testing the resonant frequency of the piezoelectric ceramic at-40-85 ℃ by using an impedance analyzer, and calculating the change rate;
s12: testing resonance point amplitude
And (5) bonding the piezoelectric ceramic plate of S10 with the metal substrate, assembling the piezoelectric vibrator, and testing the amplitude of the vibrator at the resonance point.
Further, the silver firing step in S9 is that the piezoelectric ceramic piece sintered in S8 is polished to the thickness of 0.1mm, silver paste is printed on the upper surface and the lower surface of the piezoelectric ceramic piece by adopting a screen printing process, the piezoelectric ceramic piece is placed in a heating furnace, the temperature is raised to 800 ℃, the temperature is kept for 12min, and the piezoelectric ceramic piece is naturally cooled to the room temperature; the polarization temperature in the S10 is 100-140 ℃, the polarization time is 30min, and the polarization electric field is 2-3.5 KV/mm.
By adopting the technical scheme, the invention has the following beneficial effects:
(1) on the basis of the traditional piezoelectric ceramic main body formula, a proper amount of dielectric components with perovskite structures are doped, so that the dielectric constant of the whole ceramic is improved, the electricity storage capacity of the material is enhanced, the volume of a capacitor is reduced, and the miniaturization of electrical equipment is promoted.
(2) Adding La0.1Bi0.9FeO3The method effectively inhibits crystal growth, effectively reduces the sintering temperature of the system, increases the density of the ceramic, and effectively improves the Curie temperature of the system, so that the system can adapt to higher working temperature, and the application scene of the material is widened.
(3) The planar electromechanical coupling coefficient (Kp) of the material is improved, the mechanical quality factor (Qm) value of the material is increased, the conversion efficiency between the mechanical energy and the electric energy of the material is improved, the energy consumption for overcoming the internal friction in the resonance process of the piezoelectric body is reduced, the mechanical loss is reduced, and the energy conversion efficiency is greatly improved.
(4) The displacement of the material is increased, the precision is improved to some extent, and the sensitivity of the sensor is favorably improved.
Detailed Description
In order to better understand the above technical solutions, the following detailed descriptions will be provided with reference to specific embodiments.
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
(example 1)
The doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material of the present example has a composition of xPb (Mn)1/3Nb2/3)]O3-(1-x)Pb(Zr0.52Ti0.48)]O3-ywt％Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3-zwt％La0.1Bi0.9FeO3Wherein x is 0.05, y is 2, and z is in the range of 0.2.
The preparation method of the doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material comprises the following steps:
s1: preparation of Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3Pre-sintered powder
According to the formula Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3Weighing analytically pure BaCO3、SrCO3、SnO2、Mg2(OH)2CO3、TiO2、ZrO2Powder, mixing and ball-milling the raw materials for 6-8 hours under the condition of taking ethanol as a dispersing agent, and drying to obtain a precursor of the reaction; then placing the mixed powder into an alumina crucible for presintering at 1050 ℃ for 2h, and then ball-milling for 6h to obtain Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3Pre-burning the powder;
s2: preparation of La0.1Bi0.9FeO3Pre-sintered powder
According to the formula La0.1Bi0.9FeO3Weighing analytically pure Bi2O3、Fe2O3Powder prepared by mixing the above raw materials under dispersant conditionBall milling is carried out for 6-8h, and a reaction precursor is obtained after drying; then placing the mixed powder into an alumina crucible for presintering at the presintering temperature of 900 ℃ for 2h, and then ball-milling and crushing for 6h to obtain La0.1Bi0.9FeO3Pre-burning the powder;
s3: ingredients
Raw materials are mixed according to a composition formula
xPb(Mn1/3Nb2/3)]O3-(1-x)Pb(Zr0.52Ti0.48)]O3-ywt％Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3-zwt％La0.1Bi0.9FeO3Weighing Pb3O4、MnO2、Nb2O5、ZrO2、TiO2Compounding, wherein x is 0.05, y is 2, and z is 0.2, and Ba accounting for 2 wt% of the main component is taken0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3And 0.2 wt% of La0.1Bi0.9FeO3(ii) a In which Pb is3O4The Ba is chemically pure, and other raw materials are analytically pure0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3And La0.1Bi0.9FeO3The method is obtained by synthesizing the S1 and the S2, and mixing and ball-milling the raw materials in a ball-milling tank, wherein the ball: material preparation: water is 2:1:0.5, the ball milling time is 6-8h, and then the raw materials are dried to prepare a mixture;
s4: synthesis of
Putting the dried powder of S3 into an alumina crucible, compacting and compacting, covering and sealing, and then carrying out high-temperature solid phase synthesis at the synthesis temperature of 1030 ℃ for 2 hours;
s5: water milling and drying
Ball-milling and drying the synthetic material of S4 again;
s6: fine grinding
Finely grinding the dried powder of S5 to ensure that the particle size D50 is 0.3-0.6 um;
s7: shaping and plastic discharge
Adding 14-16 wt% of polyvinyl butyral, an organic solvent, a dispersing agent and a leveling agent into the fine grinding powder prepared in the S6, preparing slurry, carrying out tape casting and punching to form a wafer with the diameter of 13 mm; granulating the obtained wafer, pressing into large blocks, aging the large blocks of blanks for 48h, grinding and granulating, and sieving the particles with a 100-mesh sieve; molding the obtained sieve material under the pressure of 8-10 MPa by using a mold with the diameter of 10mm to obtain a blank with certain strength and the thickness of 2.1 mm; heating the blank to 200 ℃ at the speed of 3 ℃/min, heating the blank to 400 ℃ at the speed of 1.5 ℃/min, keeping the temperature at 400 ℃ for 30min, heating the blank to 550 ℃ at the speed of 5 ℃/min, keeping the temperature for 10min, and discharging organic matters;
s8: sintering
And (3) burying and burning the blank body of the organic matters discharged in the step S7 by adopting lead zirconate titanate powder, carrying out the reaction in a box type furnace, heating to 1240 ℃ at the heating speed of 3 ℃/min, preserving the heat for 70min, and then cooling along with the furnace to obtain the piezoelectric ceramic piece.
In order to confirm the performance of the piezoelectric ceramic piece prepared in the steps, the performance test is carried out by adopting the following steps:
s9: silver firing
Polishing the piezoelectric ceramic sheet sintered in the step S8 to the thickness of 0.1mm, printing silver paste on the upper surface and the lower surface of the piezoelectric ceramic sheet by adopting a screen printing process, placing the piezoelectric ceramic sheet in a heating furnace, heating to 800 ℃, preserving heat for 12min, and naturally cooling to room temperature;
s10: polarization of
Polarizing the calcined silver product of S9 at 120 deg.C for 30min and with a polarizing electric field of 2.5 KV/mm;
s11: testing piezoelectric performance
Standing the piezoelectric ceramic sheet subjected to S10 polarization treatment at room temperature for 24h, testing the piezoelectric performance of the piezoelectric ceramic sheet, testing the resonant frequency of the piezoelectric ceramic at-40-85 ℃ by using an impedance analyzer, and calculating the change rate;
s12: testing resonance point amplitude
And (5) bonding the piezoelectric ceramic plate of S10 with the metal substrate, assembling the piezoelectric vibrator, and testing the amplitude of the vibrator at the resonance point.
The data test results of this example are shown in table 1.
(example 2)
This embodiment is substantially the same as embodiment 1, except that: the preparation method of the doped lead manganous niobate-lead zirconate titanate piezoelectric ceramic material of the embodiment comprises the following steps:
s3: ingredients
Raw materials are mixed according to a composition formula
xPb(Mn1/3Nb2/3)]O3-(1-x)Pb(Zr0.52Ti0.48)]O3-ywt％Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3-zwt％La0.1Bi0.9FeO3Weighing Pb3O4、MnO2、Nb2O5、ZrO2、TiO2Compounding, wherein x is 0.06, y is 0.6, z is 0.3, and Ba accounting for 0.6 wt% of the main component is taken0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3And 0.3 wt% of La0.1Bi0.9FeO3(ii) a In which Pb is3O4The Ba is chemically pure, and other raw materials are analytically pure0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3And La0.1Bi0.9FeO3The method is obtained by synthesizing the S1 and the S2, and mixing and ball-milling the raw materials in a ball-milling tank, wherein the ball: material preparation: water is 2:1:0.5, the ball milling time is 6-8h, and then the raw materials are dried to prepare a mixture;
s4: synthesis of
Putting the dried powder of S3 into an alumina crucible, compacting and compacting, covering and sealing, and then carrying out high-temperature solid phase synthesis at the synthesis temperature of 950 ℃ for 2 hours;
s8: sintering
And (3) burying and burning the blank body of the organic matters discharged in the step (S7) by adopting lead zirconate titanate powder, carrying out the reaction in a box type furnace, heating to 1220 ℃ at the heating speed of 3 ℃/min, preserving the heat for 70min, and then cooling along with the furnace to obtain the piezoelectric ceramic piece.
The data test results of this example are shown in table 2.
(comparative experiment)
Conventional xPb (Mn)1/3Nb2/3)]O3-(1-x)Pb(Zr0.52Ti0.48)]O3The piezoelectric performance test, the frequency-temperature characteristic and the vibrator resonance displacement test data are shown in table 3.
Table 1 piezoelectric performance test, frequency-temperature characteristics and resonator resonance displacement of example 1
Figure BDA0003357574070000071
Table 2 piezoelectric performance test, frequency-temperature characteristics and resonator resonance displacement of example 2
Figure BDA0003357574070000072
TABLE 3 conventional xpB (Mn)1/3Nb2/3)]O3-(1-x)Pb(Zr0.52Ti0.48)]O3Piezoelectric performance test, frequency temperature characteristic and vibrator resonance displacement
Figure BDA0003357574070000073
As can be seen from tables 1 to 3:
in example 1, the obtained piezoelectric ceramic material has a coupling coefficient Kp of 0.651-0.659, a relative dielectric constant of 1489-1517, a piezoelectric constant d33 of 349-355, a mechanical quality factor of 488-506, a loss range of 0.69-0.71, a Curie temperature of 321-329, a (-0.22% -0.11%) frequency-temperature variation range at (-40 ℃ -85 ℃), and a displacement of 34-36.
In example 2, the coupling coefficient Kp of the obtained piezoceramic material is 0.629-0.634, the relative dielectric constant is 1308-1378, the piezoelectric constant d33 is 338-343, the mechanical quality factor is 547-579, the loss range is 0.55-0.58, the Curie temperature is 331-334, the temperature variation range of the internal frequency (-0.21% -0.12%) is (-40 ℃ -85 ℃), and the displacement is 37-39.
Also, Table 3 shows that conventional xpB (Mn)1/3Nb2/3)]O3-(1-x)Pb(Zr0.52Ti0.48)]O3(x ranges from 0.04 to 0.06), the coupling coefficient Kp of the prepared piezoelectric ceramic material is 0.601 to 0.609, the relative dielectric constant is 1198 to 1221, the piezoelectric constant d33 is 319 to 322, the mechanical quality factor is 468488, the loss range is 0.55 to 0.58, the Curie temperature is 319 to 322, the temperature change interval of the internal frequency at (-40 to 85 ℃) is (-0.42 to 0.33 percent), and the displacement is 30 to 33.
Comparing the above data, it can be seen that the addition of Ba was changed0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3And the amount of La0.1Bi0.9FeO3, and the temperature in the synthesis and sintering processes are controlled, so that various parameters of the prepared piezoelectric ceramic can be effectively controlled, and the performance of the piezoelectric ceramic is relative to that of the traditional xPb (Mn)1/3Nb2/3)]O3-(1-x)Pb(Zr0.52Ti0.48)]O3(x ranges from 0.04 to 0.06) is improved. The planar electromechanical coupling coefficient of the improved material is increased, and the conversion efficiency between mechanical energy and electric energy is improved; the relative dielectric constant is increased, and the electricity storage capacity of the material is improved; the piezoelectric constant D33 is increased, and the piezoelectric performance is obviously improved; the mechanical quality factor (Qm) is increased, the energy consumed by the piezoelectric body to overcome internal friction during resonance is reduced, and the mechanical loss of the piezoelectric material is reduced; after doping, the Curie temperature is increased to some extent, and the temperature adaptation range is wider; its displacement is increased and its sensitivity to voltage changes is increased.
Therefore, compared with the traditional formula, the piezoelectric ceramic material prepared by the scheme has the advantages of greatly improved performance, higher precision and energy efficiency, and wider application occasions in various application fields.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material is characterized in that: the stoichiometric formula is xPb (Mn)1/3Nb2/3)]O3-(1-x)Pb(Zr0.52Ti0.48)]O3-ywt％Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3-zwt％La0.1Bi0.9FeO3Wherein the value range of x is 0.04-0.06, the value range of y is 0.5-3, and the value range of z is 0.1-0.3.
2. The method for preparing the doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material according to claim 1, which is characterized in that: the preparation method comprises the following preparation steps:
s1: preparation of Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3Pre-sintered powder
According to the formula Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3Weighing analytically pure BaCO3、SrCO3、SnO2、Mg2(OH)2CO3、TiO2、ZrO2Powder, performing first ball milling on the raw materials under the condition of taking ethanol as a dispersing agent, and drying to obtain a precursor of the reaction; then putting the mixed powder into an alumina crucible for pre-sintering, and then carrying out secondary ball milling to obtain Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3Pre-burning the powder;
s2: preparation of La0.1Bi0.9FeO3Pre-sintered powder
According to the formula La0.1Bi0.9FeO3Weighing analytically pure Bi2O3、Fe2O3Mixing the raw materials under the condition of a dispersing agent, performing primary ball milling, and drying to obtain a precursor of the reaction; then placing the mixed powder into an alumina crucible for presintering, and then carrying out ball milling and crushing to obtain La0.1Bi0.9FeO3Pre-burning the powder;
s3: ingredients
Raw materials are expressed by a composition formula xPb (Mn)1/3Nb2/3)]O3-(1-x)Pb(Zr0.52Ti0.48)]O3-ywt％Ba0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3-zwt％La0.1Bi0.9FeO3Weighing Pb3O4、MnO2、Nb2O5、ZrO2、TiO2Mixing materials, wherein the value range of x is 0.04-0.06, the value range of y is 0.5-3, the value range of z is 0.1-0.3, and Ba accounting for 0.5-3 wt% of the mass ratio of the main components is weighed0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3And 0.1 to 0.3 weight percent of La0.1Bi0.9FeO3(ii) a In which Pb is3O4The Ba is chemically pure, and other raw materials are analytically pure0.96Sr0.02Mg0.02Sn0.1Zr0.05Ti0.85O3And La0.1Bi0.9FeO3Mixing the raw materials in a ball milling tank, ball milling, and drying to obtain a mixture, wherein the raw materials are obtained by synthesizing the S1 and the S2;
s4: synthesis of
Putting the dried powder of S3 into an alumina crucible, compacting and compacting, and performing high-temperature solid phase synthesis after capping and sealing;
s5: water milling and drying
Ball-milling and drying the synthetic material of S4 again;
s6: fine grinding
Finely grinding the dried powder of S5 to ensure that the particle size D50 is 0.3-0.6 um;
s7: shaping and plastic discharge
Molding the powder prepared in the step S6 to prepare a blank, and then performing plastic removal treatment;
s8: sintering
And (4) burying and burning the blank body of the organic matters discharged in the step (S7) by adopting lead zirconate titanate powder, and then cooling along with the furnace to obtain the piezoelectric ceramic piece.
3. The method for preparing the lead manganese niobate-lead zirconate titanate-doped piezoelectric ceramic material according to claim 2, wherein the method comprises the following steps: in the S1, the first ball milling time is 6-8h, and the pre-sintering temperature is 950-1050 ℃; the pre-sintering time is 2 hours, and the second ball milling time is 6 hours.
4. The method for preparing the lead manganese niobate-lead zirconate titanate-doped piezoelectric ceramic material according to claim 2, wherein the method comprises the following steps: in the step S2, the presintering temperature is 900 ℃, the presintering time is 2 hours, and the ball milling and crushing time is 6 hours.
5. The method for preparing the lead manganese niobate-lead zirconate titanate-doped piezoelectric ceramic material according to claim 2, wherein the method comprises the following steps: when the materials are mixed in the ball milling tank in the S3, the ball: material preparation: the weight ratio of water is 2:1:0.5, and the ball milling time is 6-8 h.
6. The method for preparing the lead manganese niobate-lead zirconate titanate-doped piezoelectric ceramic material according to claim 2, wherein the method comprises the following steps: and the high-temperature solid-phase synthesis temperature in the S4 is 950-1050 ℃, and the reaction time is 2 h.
7. The method for preparing the lead manganese niobate-lead zirconate titanate-doped piezoelectric ceramic material according to claim 2, wherein the method comprises the following steps: the molding and plastic-discharging process in the S7 comprises the following steps: adding 14-16 wt% of polyvinyl butyral, an organic solvent, a dispersing agent and a leveling agent into the fine ground powder obtained in the step S6 to prepare slurry for tape casting, and punching into a wafer; granulating the obtained wafer, pressing into large blocks, aging the large blocks of blanks for 48h, grinding and granulating, and sieving the particles with a 100-mesh sieve; molding the obtained sieve material under the pressure of 8-10 MPa by using a mold with the diameter of 10mm to obtain a blank with certain strength and the thickness of 2.1 mm; then heating the blank body to 200 ℃ at the speed of 3 ℃/min, then heating the blank body from 200 ℃ to 400 ℃ at the speed of 1.5 ℃/min, preserving the heat at 400 ℃ for 30min, then heating the blank body to 550 ℃ at the speed of 5 ℃/min, preserving the heat for 10min, and discharging organic matters.
8. The method for preparing the lead manganese niobate-lead zirconate titanate-doped piezoelectric ceramic material according to claim 2, wherein the method comprises the following steps: and (3) carrying out the embedding burning in the S8 in a box type furnace, wherein the heating rate is 3 ℃/min, the final temperature is 1200-1250 ℃, and the heat preservation time is 70 min.
9. The method for preparing the lead manganese niobate-lead zirconate titanate-doped piezoelectric ceramic material according to claim 2, wherein the method comprises the following steps: the method also comprises the following testing steps:
s9: silver firing
Carrying out silver firing treatment on the sintered piezoelectric ceramic sheet in the S8;
s10: polarization of
Polarizing the silver-fired product of S9 under specified conditions;
s11: testing piezoelectric performance
Standing the piezoelectric ceramic sheet subjected to S10 polarization treatment at room temperature for 24h, testing the piezoelectric performance of the piezoelectric ceramic sheet, testing the resonant frequency of the piezoelectric ceramic at-40-85 ℃ by using an impedance analyzer, and calculating the change rate;
s12: testing resonance point amplitude
And (5) bonding the piezoelectric ceramic plate of S10 with the metal substrate, assembling the piezoelectric vibrator, and testing the amplitude of the vibrator at the resonance point.
10. The method for preparing the lead manganese niobate-lead zirconate titanate-doped piezoelectric ceramic material according to claim 2, wherein the method comprises the following steps:
the step of silver firing in the step S9 is that the piezoelectric ceramic piece sintered in the step S8 is polished to the thickness of 0.1mm, silver paste is printed on the upper surface and the lower surface of the piezoelectric ceramic piece by adopting a screen printing process, the piezoelectric ceramic piece is placed in a heating furnace, the temperature is raised to 800 ℃, the temperature is kept for 12min, and the piezoelectric ceramic piece is naturally cooled to the room temperature; the polarization temperature in the S10 is 100-140 ℃, the polarization time is 30min, and the polarization electric field is 2-3.5 KV/mm.
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