CN110845236A - Ta-doped potassium-sodium niobate-based piezoelectric ceramic material and preparation method thereof - Google Patents

Ta-doped potassium-sodium niobate-based piezoelectric ceramic material and preparation method thereof Download PDF

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CN110845236A
CN110845236A CN201911159114.XA CN201911159114A CN110845236A CN 110845236 A CN110845236 A CN 110845236A CN 201911159114 A CN201911159114 A CN 201911159114A CN 110845236 A CN110845236 A CN 110845236A
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袁爱桃
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Xia Lu
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Abstract

The invention provides a Ta-doped potassium-sodium niobate-based piezoelectric ceramic material and a preparation method thereof, wherein the general formula of the piezoelectric ceramic material is Na0.5K0.5Nb1‑yTayO3Wherein y is more than or equal to 0.11 and less than or equal to 0.2, the invention discloses a preparation method of the piezoceramic material, and Na is synthesized by microwave hydrothermal synthesis0.5K0.5Nb1‑yTayO3Powder, 7mol/L NaOH and KOH mixed alkali liquor as solvent, Na+And K+In a ratio of 1:6, Nb2O5And Ta2O5As a reactant, Nb2O5And Ta2O5The mass mol ratio of the total amount of the Nb to the solvent is 1: 8-1: 12, and Nb is2O5And Ta2O5The mass molar ratio of (A) to (B) is 8:1 to 4:1, inThe adding amount of the powder is 1.5 wt%, the microwave reaction temperature is 160-180 ℃, and the reaction time is 2-4 h. The invention also discloses a preparation method for preparing piezoelectric ceramics by spark sintering by using the powder, and the piezoelectric ceramics obtained by annealing treatment in oxygen atmosphere has better electrical properties.

Description

Ta-doped potassium-sodium niobate-based piezoelectric ceramic material and preparation method thereof
Technical Field
The invention relates to the technical field of functional ceramic materials, in particular to a preparation method of a Ta-doped potassium sodium niobate-based piezoelectric ceramic material.
Background
The piezoelectric ceramic is an information functional ceramic material capable of converting mechanical energy and electric energy into each other, and is widely applied to the fields of medical imaging, acoustic sensors, acoustic transducers, ultrasonic motors and the like.
Piezoelectric currently in commercial useCeramics are mainly lead-based PZT, PMNT and PZNT, and the use of these materials in large quantities can bring great harm to human life and natural environment. American scholars studied KNbO in 19593-NaNbO3When the composition is K0.5Na0.5NbO3(NKN for short), the ceramic solid solution has the best properties. KNbO3And K0.5Na0.5NbO3The phase stability temperature of the ceramic is 1040 ℃ and 1140 ℃, respectively, and the ceramic is difficult to form compact under the traditional sintering process.
Hydrothermal method (also called hydrothermal method) is a method for preparing research materials in a supercritical fluid state under the conditions of high temperature (more than 100 ℃) and high pressure (more than 9.81MPa) by using aqueous solution (or other fluids) as a reaction medium in a special closed reaction container (autoclave). The microwave hydrothermal method is introduced as a new technology for synthesizing the nano material on the basis of the hydrothermal method because the microwave hydrothermal method has incomparable advantages compared with other methods: the heating speed is high, and the material with high purity, fine strength and uniform distribution can be synthesized in a short time and at a low temperature; the sample with a certain depth can be directly penetrated, and the heating is carried out at different depths simultaneously, so that the heating is rapid and uniform; by adjusting the output power of the microwave, the sample can be immediately and inertlessly changed under the heating condition, so that automatic control and continuous operation are facilitated; the heat energy utilization rate is high, and the energy can be greatly saved. At present, some metal oxide nano powder is successfully synthesized by a microwave hydrothermal method.
CN102351536A provides a method for preparing potassium sodium niobate-based powder and piezoelectric ceramic thereof by microwave hydrothermal synthesis, which takes KOH and NaOH mixed alkali liquor as a reaction solvent, NaOH: KOH 1.3 to 1.5:4.5 to 4.7 and Nb2O5Doping LiTaO as reactant3Microwave hydrothermal synthesis of KxNa1-x-yNb1-yO3—yLiTaO3After the powder is prepared, the piezoelectric ceramic is finally obtained through PVA granulation, compression molding, plastic removal, normal-pressure sintering and polarization. Compactness is to pressingThe performance of the piezoelectric ceramic is greatly influenced, the problem of the density of the sintered ceramic is not researched by the scheme, and the density of the piezoelectric ceramic is not improved by taking measures, so that the electrical and mechanical properties of the piezoelectric ceramic cannot be greatly improved.
Disclosure of Invention
Aiming at the problems in the prior art, the application provides a Ta-doped potassium sodium niobate-based piezoelectric ceramic material Na0.5K0.5Nb1-yTayO3And a method for preparing the same. The relative density of the piezoelectric ceramic prepared by the invention is more than 95%, the relative dielectric constant is 1129-1141, the piezoelectric constant is 262-270, and the dielectric loss is reduced to 0.014-0.016.
The technical scheme of the invention is as follows:
1.Na0.5K0.5Nb1-yTayO3preparing powder:
(1) adding water into solid NaOH and KOH to prepare mixed alkali liquor with the concentration of 7mol/L as a solvent, wherein Na is+And K+In a ratio of 1:6, Nb2O5And Ta2O5The mass molar ratio of the total addition amount of the Nb to the solvent is 1: 8-1: 12, wherein Nb is2O5And Ta2O5The mass molar ratio of (1) to (4) is 8:1 to 1, and 1.5 wt% of a dispersant is added.
(2) And mixing, placing the mixture into a polytetrafluoroethylene lining reaction kettle, placing the reaction kettle into a microwave reactor, setting the reaction temperature to be 160-180 ℃, and reacting for 2-4 hours.
(3) After the reaction is completed, white precipitate can be seen at the bottom of the lining, and the supernatant of the lining is poured into a beaker and is dripped with hydrochloric acid until no precipitate is seen in the neutral state, which indicates that no soluble niobate and tantalate exist in the solution.
(4) The white precipitate at the bottom of the liner was washed to neutrality with deionized water and dried in an oven at 100 ℃ for 1 h.
2.Na0.5K0.5Nb1-yTayO3Preparing piezoelectric ceramics:
(1) adding 8-10% of polyvinyl alcohol (PVA) into the powder prepared by the microwave hydrothermal method according to mass percent for granulation, prepressing and molding under the pressure of 40-50 Mpa, and carrying out cold isostatic pressing and molding under the pressure of 180-230 Mpa.
(2) Keeping the temperature at 500-600 ℃ for 30-50 min to remove PVA, and raising the temperature at 5 ℃/min.
(3) Plasma spark sintering, wherein the axial pressure is 60MPa, the sintering temperature is 870-910 ℃, the sintering time is 4-8 min, annealing treatment is carried out in an oxygen atmosphere, the oxygen flow is 4ml/min, the temperature rising speed is 4 ℃/min, the temperature is raised to 500 ℃, and the temperature is kept for 3-4 h; the oxygen flow is 2ml/min, the heating rate is 4 ℃/min, the temperature is increased to 800 ℃, the temperature is kept for 2-3 h, and the temperature is naturally reduced to the room temperature.
(4) And (3) insulating the sintered ceramic sample at 700 ℃ for 0.5h, polarizing after silver plating, wherein the polarizing temperature is 120-150 ℃, the polarizing electric field is 4-7 kv/m, and the polarizing time is 15-25 min.
Preferably, the dispersant is polyethylene glycol, polyacrylic acid, polycarboxylate ether.
Na0.5K0.5Nb1-yTayO3Ta source of (1) selecting Ta2O5As a reactant other than LiTaO3The reason is that Li is easy to volatilize in the sintering process, and influences the compactness of the ceramic.
Na prepared by microwave hydrothermal method can be effectively inhibited by adding dispersing agent0.5K0.5Nb1-yTayO3The superfine powder is obtained by the agglomeration of the powder, the advantages of the superfine powder can be better exerted in the later powder forming and sintering processes, and the polyethylene glycol, the polyacrylic acid and the polycarboxylate ether can be discharged at 400-500 degrees without influencing the later sintering.
The invention has the beneficial effects that:
the invention provides a Ta-doped potassium-sodium niobate-based piezoelectric ceramic material and a preparation method thereof, which adopts a microwave hydrothermal method to synthesize early-stage powder, has low reaction temperature, short time and high heat energy utilization rate, and selects Ta2O5As a reactant other than LiTaO3The reason is that Li is easily volatilized during sintering, and gaseous Li2O is easy to dissociate with LiTaO along with air hole3Generation of Li3TaO4。
The polyethylene glycol, polyacrylic acid and polycarboxylate ether dispersing agent can inhibit the agglomeration of powder synthesized by microwave hydrothermal synthesis, the dispersing agent forms chain molecules after being dissociated in water, space bit group action is generated after the dispersing agent is adsorbed on the surface of powder particles, collision and aggregation are hindered, the dispersion stability is enhanced, necessary conditions are provided for the compactness of later-stage sintered ceramics after the superfine powder is obtained, and the cold isostatic pressing is adopted, so that the uniform pressure in all directions can be ensured, and the density difference is reduced. The plasma spark sintering has the advantages of high temperature rising speed, low sintering temperature, high sintering efficiency and high density of the ceramic matrix.
The reduction of the oxygen vacancy concentration can improve the electrical property of the piezoelectric ceramic, and the mechanism is that the oxygen vacancies have higher migration rate, an internal electric field opposite to the direction of a loading electric field is formed under the driving of an external electric field, the internal electric field obstructs wall movement, so that the dielectric loss is increased, the dielectric constant is reduced, the oxygen vacancy concentration can be effectively reduced by annealing in the oxygen atmosphere, new defect distribution can be increased by too high oxygen flow, the oxygen vacancy defect can be effectively repaired by controlling the oxygen flow, and finally, the prepared piezoelectric ceramic has better electrical property.
Description of the drawings:
FIG. 1 is Na0.5K0.5NbO3Powder XRD spectrum;
FIG. 2 shows Na in example I0.5K0.5Nb0.89Ta0.11O3Powder XRD spectrum;
FIG. 3 shows Na in example II0.5K0.5Nb0.86Ta0.14O3Powder XRD spectrum;
FIG. 4 shows Na in example III0.5K0.5Nb0.83Ta0.17O3Powder XRD spectrum;
FIG. 5 shows Na in example IV0.5K0.5Nb0.8Ta0.2O3Powder XRD pattern.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
1.Na0.5K0.5Nb0.89Ta0.11O3preparing powder:
(1) adding water into solid KOH and NaOH to prepare mixed alkali liquor with the concentration of 7mol/L and Na+And K+In a ratio of 1:6, respectively, Nb2O5And Ta2O5The mass molar ratio of the total addition amount of the Nb to the alkali liquor is 1:8, wherein the Nb is2O5And Ta2O5The mass molar ratio of (1) to (2) is 8:1, and 1.5 wt% of polyethylene glycol is added.
(2) Mixing the powder with alkali liquor, placing the mixture into a reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle into a microwave reactor, setting the reaction temperature to be 160 ℃, and reacting for 2 hours.
(3) Pouring the supernatant of the lining into a beaker, and dropwise adding hydrochloric acid until the supernatant is neutral, wherein no precipitate is generated.
(4) The white precipitate at the bottom of the liner was washed to neutrality with deionized water and dried in an oven at 100 ℃ for 1 h.
2.Na0.5K0.5Nb1-yTayO3Preparing piezoelectric ceramics:
(1) adding 8% polyvinyl alcohol (PVA) into the powder prepared by the microwave hydrothermal method according to mass percent for granulation, prepressing and molding under the pressure of 40Mpa, and carrying out cold isostatic pressing and molding under the pressure of 200 Mpa.
(2) Keeping the temperature at 600 ℃ for 30min to remove PVA, and the heating rate is 5 ℃/min.
(3) Plasma spark sintering, wherein the axial pressure is 60MPa, the sintering temperature is 880 ℃, the sintering time is 6min, annealing treatment is carried out in an oxygen atmosphere, the oxygen flow is 4ml/min, the temperature rise speed is 4 ℃/min, the temperature is raised to 500 ℃, and the temperature is kept for 3 h; the oxygen flow is 2ml/min, the heating rate is 4 ℃/min, the temperature is raised to 800 ℃, the temperature is kept for 2h, and the temperature is naturally reduced to the room temperature.
(4) And (3) carrying out heat preservation on the sintered ceramic at 700 ℃ for 0.5h, polarizing after silver plating, wherein the polarizing temperature is 130 ℃, the polarizing electric field is 6kv/m, and the polarizing time is 20 min.
Na prepared in this example0.5K0.5Nb0.89Ta0.11O3XRD pattern (shown in figure 2) and figure 1Na0.5K0.5NbO3The main crystal phase in the XRD pattern is consistent.
Example 2:
1.Na0.5K0.5Nb0.86Ta0.14O3preparing powder:
(1) adding water into solid KOH and NaOH to prepare mixed alkali liquor with the concentration of 7mol/L, wherein Na is contained in the mixed alkali liquor+And K+In a ratio of 1:6, respectively, Nb2O5And Ta2O5The mass molar ratio of the total addition amount of the Nb to the alkali liquor is 1:8, wherein the Nb is2O5And Ta2O5The mass molar ratio of (2) is 6:1, and polyacrylic acid is added in an amount of 1.5 wt%.
(2) Mixing the powder with alkali liquor, placing the mixture into a reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle into a microwave reactor, setting the reaction temperature to be 170 ℃, and reacting for 3 hours.
(3) Pouring the supernatant of the lining into a beaker, and dropwise adding hydrochloric acid until the supernatant is neutral, wherein no precipitate is generated.
(4) The white precipitate at the bottom of the liner was washed to neutrality with deionized water and dried in an oven at 100 ℃ for 1 h.
2.Na0.5K0.5Nb1-yTayO3Preparing piezoelectric ceramics:
(1) adding 8% polyvinyl alcohol (PVA) into the powder prepared by the microwave hydrothermal method according to mass percent for granulation, prepressing and molding under the pressure of 40Mpa, and carrying out cold isostatic pressing and molding under the pressure of 210 Mpa.
(2) Keeping the temperature at 500 ℃ for 40min to remove PVA, and the heating rate is 5 ℃/min.
(3) Plasma spark sintering, wherein the axial pressure is 60MPa, the sintering temperature is 890 ℃, the sintering time is 5min, annealing treatment is carried out in an oxygen atmosphere, the oxygen flow is 4ml/min, the temperature rising speed is 4 ℃/min, the temperature is raised to 500 ℃, and the temperature is preserved for 3.5 h; the oxygen flow is 2ml/min, the heating rate is 4 ℃/min, the temperature is raised to 800 ℃, the temperature is kept for 2h, and the temperature is naturally reduced to the room temperature.
(4) And (3) carrying out heat preservation on the sintered ceramic at 700 ℃ for 0.5h, polarizing after silver plating, wherein the polarizing temperature is 130 ℃, the polarizing electric field is 5kv/m, and the polarizing time is 25 min.
Na prepared in this example0.5K0.5Nb0.86Ta0.14O3XRD pattern (shown in figure 3) and figure 1Na0.5K0.5NbO3The main crystal phase in the XRD pattern is consistent.
Example 3:
1.Na0.5K0.5Nb0.83Ta0.17O3preparing powder:
(1) adding water into solid KOH and NaOH to prepare mixed alkali liquor with the concentration of 7mol/L, wherein Na is contained in the mixed alkali liquor+And K+In a ratio of 1:6, respectively, Nb2O5And Ta2O5The mass molar ratio of the total addition amount of the Nb to the alkali liquor is 1:10, wherein the Nb is2O5And Ta2O5The mass molar ratio of (1) to (2) is 5:1, and polyacrylic acid is added in an amount of 1.5 wt%.
(2) Mixing the powder with alkali liquor, placing the mixture into a reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle into a microwave reactor, setting the reaction temperature to be 180 ℃, and reacting for 3 hours.
(3) Pouring the supernatant of the lining into a beaker, and dropwise adding hydrochloric acid until the supernatant is neutral, wherein no precipitate is generated.
(4) The white precipitate at the bottom of the liner was washed to neutrality with deionized water and dried in an oven at 100 ℃ for 1 h.
2.Na0.5K0.5Nb1-yTayO3Preparing piezoelectric ceramics:
(1) adding 8% polyvinyl alcohol (PVA) into the powder prepared by the microwave hydrothermal method according to mass percent for granulation, prepressing and molding under the pressure of 50MPa, and carrying out cold isostatic pressing and molding under the pressure of 200 MPa.
(2) Keeping the temperature at 500 ℃ for 40min to remove PVA, and the heating rate is 5 ℃/min.
(3) Plasma spark sintering, wherein the axial pressure is 60MPa, the sintering temperature is 910 ℃, the sintering time is 5min, annealing treatment is carried out in an oxygen atmosphere, the oxygen flow is 4ml/min, the heating rate is 4 ℃/min, the temperature is increased to 500 ℃, and the temperature is kept for 4 h; the oxygen flow is 2ml/min, the heating rate is 4 ℃/min, the temperature is increased to 800 ℃, the temperature is kept for 2.5h, and the temperature is naturally reduced to the room temperature.
(4) And (3) carrying out heat preservation on the sintered ceramic at 700 ℃ for 0.5h, polarizing after silver plating, wherein the polarizing temperature is 140 ℃, the polarizing electric field is 5kv/m, and the polarizing time is 25 min.
Na prepared in this example0.5K0.5Nb0.83Ta0.17O3XRD pattern (shown in figure 4) and figure 1Na0.5K0.5NbO3The main crystal phase in the XRD pattern is consistent.
Example 4:
1.Na0.5K0.5Nb0.8Ta0.2O3preparing powder:
(1) adding water into solid KOH and NaOH to prepare mixed alkali liquor with the concentration of 7mol/L, wherein Na is contained in the mixed alkali liquor+And K+In a ratio of 1:6, respectively, Nb2O5And Ta2O5The mass molar ratio of the total addition amount of the Nb to the alkali liquor is 1:10, wherein the Nb is2O5And Ta2O5The mass molar ratio of (1) was 4:1, and 1.5 wt% of polycarboxylate ether was added.
(2) Mixing the powder with alkali liquor, placing the mixture into a reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle into a microwave reactor, setting the reaction temperature to be 170 ℃, and reacting for 4 hours.
(3) Pouring the supernatant of the lining into a beaker, and dropwise adding hydrochloric acid until the supernatant is neutral, wherein no precipitate is generated.
(4) The white precipitate at the bottom of the liner was washed to neutrality with deionized water and dried in an oven at 100 ℃ for 1 h.
2. Piezoelectric ceramic sample preparation:
(1) adding 8% polyvinyl alcohol (PVA) into the powder prepared by the microwave hydrothermal method according to mass percent for granulation, prepressing and molding under the pressure of 50MPa, and carrying out cold isostatic pressing and molding under the pressure of 200 MPa.
(2) Keeping the temperature at 500 ℃ for 40min to remove PVA, and the heating rate is 5 ℃/min.
(3) Plasma spark sintering, wherein the axial pressure is 60MPa, the sintering temperature is 890 ℃, the sintering time is 7min, annealing treatment is carried out in an oxygen atmosphere, the oxygen flow is 4ml/min, the temperature rising speed is 4 ℃/min, the temperature is raised to 500 ℃, and the temperature is preserved for 3.5 h; the oxygen flow is 2ml/min, the heating rate is 4 ℃/min, the temperature is increased to 800 ℃, the temperature is kept for 2.5h, and the temperature is naturally reduced to the room temperature.
(4) And (3) carrying out heat preservation on the sintered ceramic at 700 ℃ for 0.5h, polarizing after silver plating, wherein the polarizing temperature is 150 ℃, the polarizing electric field is 5kv/m, and the polarizing time is 25 min.
Na prepared in this example0.5K0.5Nb0.8Ta0.2O3XRD pattern (shown in figure 5) and figure 1Na0.5K0.5NbO3The main crystal phase in the XRD pattern is consistent.
Comparative example 1: the dispersant in example 1 was removed and the other raw materials and preparation method were the same as in example 1.
Comparative example 2: the spark sintering process in example 2 was removed and atmospheric sintering was used, and the other raw materials and preparation method were the same as in example 2.
Comparative example 3: the annealing treatment process under the oxidizing atmosphere in example 3 was removed, and other raw materials and preparation methods were the same as those in example 3.
Comparative example 4: the oxygen flow rates in the first and second temperature rise stages of the annealing process under the oxidizing atmosphere in example 3 were set to 6ml/min and 2ml/min, respectively, and the other raw materials and preparation methods were the same as in example 3.
Comparative example 5: the oxygen flow rates in the first and second temperature rise stages of the annealing process under the oxidizing atmosphere in example 4 were set to 3ml/min and 1ml/min, respectively, and the other raw materials and preparation methods were the same as those in example 3.
Comparative example 6: the oxygen flow rates in the first and second temperature rise stages of the annealing process under the oxidizing atmosphere in example 4 were set to 5ml/min and 3ml/min, respectively, and other raw materials and preparation methods were the same as those in example 4.
Comparative example 7: the oxygen flow rates in the first and second temperature rise stages of the annealing process under the oxidizing atmosphere in example 4 were set to 2ml/min and 3ml/min, respectively, and the other raw materials and preparation methods were the same as in example 4.
The piezoelectric ceramics obtained in the comparative example and the example were subjected to the performance test as shown in table 1: piezoelectric ceramic performance parameters
Figure BDA0002285581750000091
As can be seen from the data in Table 1, in comparative example 1, no dispersant is used, the early-stage powder prepared by the microwave hydrothermal method is easy to agglomerate, the advantages of the ultrafine powder cannot be exerted, and the relative density and compactness of the ceramic substrate sintered at the later stage are low, so that the performance parameters are reduced. In the comparative example 2, the ceramic substrate is sintered at normal pressure without spark, so that the relative density is low, the compactness is not high, and the performance parameters are reduced. The sintered ceramic matrix in the comparative example 3 is not subjected to an annealing process in an oxidizing atmosphere, the density of the ceramic matrix is not much different from that of the ceramic matrix in the example 3, but the sintered ceramic matrix has high oxygen vacancy concentration and high oxygen vacancy migration rate, an internal electric field opposite to the direction of a loaded electric field is formed under the driving of an external electric field, the wall of is prevented from moving by the internal electric field, so that the electrical property is poor, the annealing process in the oxidizing atmosphere in the comparative example 4 adopts 6ml/min and 2ml/min respectively, the performance parameter is poorer than that in the comparative example 3, new defect distribution can be increased due to overhigh oxygen flow, the annealing process in the oxidizing atmosphere in the comparative example 5 adopts 3ml/min and 1ml/min respectively, the performance parameter is improved compared with that in the comparative example 3, but the performance parameter does not reach the level in. Comparative example 6 has the same problems as comparative example 4, and the piezoelectric ceramic properties are deteriorated due to an excessive oxygen flow, and the piezoelectric ceramic properties are not optimal in comparative example 7.
While the embodiments of the present invention have been disclosed above, it is not limited to the applications listed in the description and embodiments, but is fully applicable to various fields suitable for the present invention, and it will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in the embodiments without departing from the principle and spirit of the present invention, and therefore the present invention is not limited to the specific details without departing from the general concept defined in the claims and the scope of equivalents thereof.

Claims (5)

1. A Ta-doped potassium sodium niobate-based piezoelectric ceramic material is characterized in that the general formula of the piezoelectric ceramic material is Na0.5K0.5Nb1-yTayO3Wherein y is more than or equal to 0.11 and less than or equal to 0.2.
2. A method for preparing Ta-doped potassium sodium niobate-based piezoelectric ceramic material is characterized by comprising the microwave hydrothermal synthesis of Na0.5K0.5Nb1-yTayO3Method for producing powder and Na0.5K0.5Nb1-yTayO3A method for preparing ceramics.
3. The method for preparing a Ta-doped potassium sodium niobate-based piezoelectric ceramic material as claimed in claim 2, wherein the microwave hydrothermal synthesis of Na is performed0.5K0.5Nb1-yTayO3The preparation method of the powder comprises the following steps: 7mol/L NaOH and KOH mixed alkali liquor is used as solvent, Na+And K+In a ratio of 1:6, Nb2O5And Ta2O5As a reactant, Nb2O5And Ta2O5The mass mol ratio of the total amount of the Nb to the solvent is 1: 8-1: 12, and Nb is2O5And Ta2O5The mass molar ratio of the dispersant to the organic solvent is 8: 1-4: 1, the addition amount of the dispersant is 1.5 wt%, the reaction temperature is 160-180 ℃, and the reaction time is 2-4 h.
4. The method for preparing a Ta-doped potassium sodium niobate-based piezoelectric ceramic material as claimed in claim 2, wherein the dispersant is polyethylene glycol, polyacrylic acid, polycarboxylate ether.
5. The method for preparing a Ta-doped potassium sodium niobate-based piezoelectric ceramic material as claimed in claim 2, wherein said Na is added0.5K0.5Nb1-yTayO3The preparation method of the ceramic comprises the following steps:
(1)Na0.5K0.5Nb1-yTayO3washing the powder to dry in an oven, adding 8-10% polyvinyl alcohol for granulation, pre-pressing and molding under the pressure of 40-50 Mpa, and cold isostatic pressing and molding under the pressure of 180-230 Mpa;
(2) keeping the temperature at 500-600 ℃ for 30-50 min to remove PVA, and raising the temperature at 5 ℃/min;
(3) plasma spark sintering, wherein the axial pressure is 60MPa, the sintering temperature is 870-910 ℃, the sintering time is 4-8 min, annealing treatment is carried out in an oxygen atmosphere, the oxygen flow is 4ml/min, the temperature rising speed is 4 ℃/min, the temperature is raised to 500 ℃, and the temperature is kept for 3-4 h; the oxygen flow is 2ml/min, the heating rate is 4 ℃/min, the temperature is increased to 800 ℃, the temperature is kept for 2-3 h, and the temperature is naturally reduced to the room temperature.
(4) And (3) insulating the sintered ceramic sample at 700 ℃ for 0.5h for silver plating polarization, wherein the polarization temperature is 120-150 ℃, the polarization electric field is 4-7 kv/m, and the polarization time is 15-25 min.
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