CN110845236B - 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 PDFInfo
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Abstract
The application 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 Na 0.5 K 0.5 Nb 1‑y Ta y O 3 Wherein y is more than or equal to 0.11 and less than or equal to 0.2, the application discloses a preparation method of the piezoelectric ceramic material, and Na is synthesized by microwave hydrothermal method 0.5 K 0.5 Nb 1‑y Ta y O 3 Powder, 7mol/L NaOH and KOH mixed alkali solution as solvent, na + And K + In a ratio of 1:6, nb 2 O 5 And Ta 2 O 5 As reactant, nb 2 O 5 And Ta 2 O 5 The mass mol ratio of the total added amount to the solvent is 1:8-1:12, nb 2 O 5 With Ta 2 O 5 The mass molar ratio of the dispersant is 8:1-4:1, the addition amount of the dispersant is 1.5wt%, the microwave reaction temperature is 160-180 ℃, and the reaction time is 2-4 h. The application also discloses a preparation method for preparing the piezoelectric ceramic by utilizing the powder through spark sintering, and the piezoelectric ceramic obtained through annealing treatment in oxygen atmosphere has better electrical property.
Description
Technical Field
The application 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 mutually converting mechanical energy and electric energy, and is widely applied to the fields of medical imaging, acoustic sensors, acoustic transducers, ultrasonic motors and the like.
The piezoelectric ceramics in the current industry are mainly lead-based PZT, PMNT and PZNT, and the large-scale use of the materials can bring great harm to human life and natural environment. The American scholars studied KNbO in 1959 3 -NaNbO 3 When the composition is K 0.5 Na 0.5 NbO 3 When (abbreviated as NKN), the ceramic solid solution has the best performance. KNbO 3 And K 0.5 Na 0.5 NbO 3 The phase stabilization temperatures of (2) are 1040 ℃ and 1140 ℃ respectively, and dense ceramics are difficult to form under the traditional sintering process.
Hydrothermal process (also called hydrothermal process) is a process for preparing research material in special closed reaction container (high-pressure reactor) under high-temp (above 100 deg.C) and high-pressure (above 9.81 MPa) condition by using aqueous solution (or other fluid) as reaction medium. The microwave hydrothermal method is introduced on the basis of the hydrothermal method as a novel technology for synthesizing the nano material, and has the advantages incomparable with other methods: the heating speed is high, and materials with high purity, fine strength and uniform distribution can be synthesized in a short time at low temperature; the sample with a certain depth can be directly penetrated, and the sample can be heated at different depths at the same time, so that the heating is quick and uniform; by adjusting the output power of the microwaves, the sample can be immediately changed without inertia under the heating condition, and the automatic control and continuous operation are convenient; the heat energy utilization rate is high, and the energy can be greatly saved. At present, a microwave hydrothermal method is used for successfully synthesizing some metal oxide nano powder.
CN102351536a provides a method for preparing potassium-sodium niobate based powder and piezoelectric ceramic by microwave hydrothermal synthesis, which uses mixed alkali solution of KOH and NaOH as reaction solvent, naOH: KOH=1.3 to 1.5:4.5 to 4.7, with Nb 2 O 5 Doped with LiTaO as reactant 3 Microwave hydro-thermal synthesis K x Na 1-x-y Nb 1-y O 3— yLiTaO 3 After the powder is prepared, the piezoelectric ceramic is finally obtained through PVA granulation, compression molding, plastic discharge, normal-pressure sintering and polarization, the preparation method shortens the time, plays the advantage of microwave synthesis, and the obtained potassium-sodium niobate-based piezoelectric ceramic has certain improvement on performance, but has no particularly good effect. The compactness has great influence on the performance of the piezoelectric ceramic, the scheme has no study on the problem of ceramic compactness after sintering, and measures are not taken to improve the compactness of the piezoelectric ceramic, so that the electrical and mechanical properties of the piezoelectric ceramic cannot be greatly improved.
Disclosure of Invention
Aiming at the problems existing in the prior art, the application provides a Ta-doped potassium-sodium niobate based piezoceramic material Na 0.5 K 0.5 Nb 1-y Ta y O 3 And a method for preparing the same. The piezoelectric ceramic prepared by the application has the relative density of more than 95%, the relative dielectric constant of 1129-1141, the piezoelectric constant of 262-270 and the dielectric loss of 0.014-0.016.
The technical scheme of the application is as follows:
1.Na 0.5 K 0.5 Nb 1-y Ta y O 3 preparing 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 + And K + In a ratio of 1:6, nb 2 O 5 And Ta 2 O 5 The mass mol ratio of the added total amount of (2) to the solvent is 1:8-1:12, wherein Nb 2 O 5 And Ta 2 O 5 The mass mol ratio of (2) is 8:1-4:1, and 1.5wt% of dispersing agent is added.
(2) Mixing and then 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 the reaction time to be 2-4 h.
(3) After the reaction was completed, a white precipitate was visible at the bottom of the liner, and the supernatant of the liner was poured into a beaker and added dropwise with hydrochloric acid until no precipitate was formed to neutrality, indicating that there was no soluble niobate or tantalate 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 1h.
2.Na 0.5 K 0.5 Nb 1-y Ta y O 3 Piezoelectric ceramics preparation:
(1) Adding 8-10% polyvinyl alcohol (PVA) into the powder prepared by a microwave hydrothermal method according to the mass percentage, granulating, prepressing and forming under the pressure of 40-50 Mpa, and cold isostatic pressing and forming under the pressure of 180-230 Mpa.
(2) Preserving the temperature at 500-600 ℃ for 30-50 min to remove PVA, wherein the temperature rising speed is 5 ℃/min.
(3) Plasma spark sintering, axial pressure of 60MPa, sintering temperature of 870-910 ℃, sintering time of 4-8 min, annealing treatment in oxygen atmosphere, oxygen flow of 4ml/min, heating speed of 4 ℃/min, heating to 500 ℃, and heat preservation for 3-4 h; oxygen flow rate is 2ml/min, heating speed is 4 ℃/min, heating to 800 ℃, preserving heat for 2-3 h, and naturally cooling to room temperature.
(4) The sintered ceramic sample is subjected to silver plating at 700 ℃ for 0.5h and then polarized, the polarization temperature is 120-150 ℃, the polarization electric field is 4-7 kv/m, and the polarization time is 15-25 min.
Preferably, the dispersing agent is polyethylene glycol, polyacrylic acid or polycarboxylate ether.
Na 0.5 K 0.5 Nb 1-y Ta y O 3 Ta source selection Ta in (a) 2 O 5 As reactants other than LiTaO 3 The reason is that Li is easily volatilized during sintering, which affects the density of the ceramic.
The addition of the dispersing agent can effectively inhibit Na prepared by a microwave hydrothermal method 0.5 K 0.5 Nb 1-y Ta y O 3 The powder is agglomerated to obtain superfine powder, the advantages of the superfine powder can be better played in the later powder forming and sintering process, and polyethylene glycol, polyacrylic acid and polycarboxylate ether can be discharged at 400-500, so that the later sintering is not affected.
The application has the beneficial effects that:
the application 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 utilization rate, and selects Ta 2 O 5 As reactants other than LiTaO 3 Since Li is easily volatilized during sintering, and Li in a gaseous state 2 O is free along with air holes and is easy to be combined with LiTaO 3 Li generation 3 TaO 4 。
Polyethylene glycol, polyacrylic acid and polycarboxylate ether dispersing agent can inhibit agglomeration of powder synthesized by microwave hydrothermal, and the dispersing agent forms chain molecules after being dissociated in water, generates space bit group effect after being adsorbed on the surface of powder particles, prevents collision aggregation, enhances dispersion stability, provides necessary conditions for compactness of later-stage sintered ceramic after obtaining superfine powder, and can ensure uniform pressure in all directions and reduce density difference by adopting cold isostatic pressing. Plasma spark sintering, high temperature rising speed, low sintering temperature, high sintering efficiency and high ceramic matrix density.
The reduction of the oxygen vacancy concentration can improve the electrical property of the piezoelectric ceramic, and the mechanism is that the oxygen vacancy has higher migration rate, an internal electric field opposite to the loading electric field is formed under the drive of an external electric field, the internal electric field blocks wall movement, so that dielectric loss is increased, dielectric constant is reduced, the oxygen vacancy concentration can be effectively reduced by annealing in an oxygen atmosphere, new defect distribution can be increased by excessively 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 Na 0.5 K 0.5 NbO 3 Powder XRD pattern;
FIG. 2 is Na in embodiment one 0.5 K 0.5 Nb 0.89 Ta 0.11 O 3 Powder XRD pattern;
FIG. 3 is Na in example two 0.5 K 0.5 Nb 0.86 Ta 0.14 O 3 Powder XRD pattern;
FIG. 4 is Na in example III 0.5 K 0.5 Nb 0.83 Ta 0.17 O 3 Powder XRD pattern;
FIG. 5 is Na in example IV 0.5 K 0.5 Nb 0.8 Ta 0.2 O 3 Powder XRD pattern.
Detailed Description
The present application will be described in detail below with reference to the drawings and examples. It will be apparent that the described embodiments are only some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1:
1.Na 0.5 K 0.5 Nb 0.89 Ta 0.11 O 3 preparing powder:
(1) Adding water into solid KOH and NaOH to prepare mixed alkali liquor with concentration of 7mol/L, na + And K + The ratio of Nb is 1:6 respectively 2 O 5 And Ta 2 O 5 The molar ratio of the total added amount of Nb to the alkali lye is 1:8, wherein Nb 2 O 5 And Ta 2 O 5 The mass mol ratio of (2) is 8:1, and polyethylene glycol is added in an amount of 1.5wt%.
(2) Mixing the powder with alkali liquor, placing the mixture into a polytetrafluoroethylene lining reaction kettle, placing the reaction kettle into a microwave reactor, setting the reaction temperature to 160 ℃, and reacting for 2 hours.
(3) The supernatant of the lining was poured into a beaker and hydrochloric acid was added dropwise until neutral, and no precipitate was formed.
(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 1h.
2.Na 0.5 K 0.5 Nb 1-y Ta y O 3 Piezoelectric ceramics preparation:
(1) Adding 8% polyvinyl alcohol (PVA) into the powder prepared by a microwave hydrothermal method according to the mass percentage, granulating, prepressing and forming under 40Mpa pressure, and cold isostatic pressing and forming under 200Mpa pressure.
(2) The temperature is kept at 600 ℃ for 30min to remove PVA, and the temperature rising speed is 5 ℃/min.
(3) Plasma spark sintering, axial pressure of 60MPa, sintering temperature of 880 ℃, sintering time of 6min, annealing treatment in oxygen atmosphere, oxygen flow of 4ml/min, heating speed of 4 ℃/min, heating to 500 ℃, and heat preservation for 3h; oxygen flow rate is 2ml/min, heating speed is 4 ℃/min, heating to 800 ℃, preserving heat for 2h, and naturally cooling to room temperature.
(4) The sintered ceramic is subjected to silver plating at 700 ℃ for 0.5h and then polarized, the polarization temperature is 130 ℃, the polarization electric field is 6kv/m, and the polarization time is 20min.
Na prepared in this example 0.5 K 0.5 Nb 0.89 Ta 0.11 O 3 XRD patterns (shown in FIG. 2) and FIG. 1Na 0.5 K 0.5 NbO 3 The main crystal phase in the XRD pattern is consistent.
Example 2:
1.Na 0.5 K 0.5 Nb 0.86 Ta 0.14 O 3 preparing powder:
(1) Adding water into solid KOH and NaOH to prepare mixed alkali liquor with the concentration of 7mol/L, wherein Na + And K + The ratio of Nb is 1:6 respectively 2 O 5 And Ta 2 O 5 The molar ratio of the total added amount of Nb to the alkali lye is 1:8, wherein Nb 2 O 5 And Ta 2 O 5 Quality of (2)The molar ratio was 6:1 and polyacrylic acid was added at 1.5wt%.
(2) Mixing the powder with alkali liquor, placing the mixture into a polytetrafluoroethylene lining reaction kettle, placing the reaction kettle into a microwave reactor, setting the reaction temperature to 170 ℃ and reacting for 3 hours.
(3) The supernatant of the lining was poured into a beaker and hydrochloric acid was added dropwise until neutral, and no precipitate was formed.
(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 1h.
2.Na 0.5 K 0.5 Nb 1-y Ta y O 3 Piezoelectric ceramics preparation:
(1) Adding 8% polyvinyl alcohol (PVA) into the powder prepared by a microwave hydrothermal method according to the mass percentage, granulating, prepressing and forming under 40Mpa pressure, and cold isostatic pressing and forming under 210Mpa pressure.
(2) Preserving the temperature at 500 ℃ for 40min to remove PVA, wherein the temperature rising speed is 5 ℃/min.
(3) Plasma spark sintering, axial pressure of 60MPa, sintering temperature of 890 ℃, sintering time of 5min, annealing treatment in oxygen atmosphere, oxygen flow of 4ml/min, heating speed of 4 ℃/min, heating to 500 ℃, and heat preservation for 3.5h; oxygen flow rate is 2ml/min, heating speed is 4 ℃/min, heating to 800 ℃, preserving heat for 2h, and naturally cooling to room temperature.
(4) The sintered ceramic is subjected to silver plating at 700 ℃ for 0.5h and then polarized, the polarization temperature is 130 ℃, the polarization electric field is 5kv/m, and the polarization time is 25min.
Na prepared in this example 0.5 K 0.5 Nb 0.86 Ta 0.14 O 3 XRD pattern (shown in FIG. 3) and FIG. 1Na 0.5 K 0.5 NbO 3 The main crystal phase in the XRD pattern is consistent.
Example 3:
1.Na 0.5 K 0.5 Nb 0.83 Ta 0.17 O 3 preparing powder:
(1) Adding water into solid KOH and NaOH to prepare mixed alkali liquor with the concentration of 7mol/L, wherein Na + And K + The ratio of Nb is 1:6 respectively 2 O 5 And Ta 2 O 5 Is added with (a)The mass molar ratio of the total amount to the alkali liquor is 1:10, wherein Nb 2 O 5 And Ta 2 O 5 The mass molar ratio of (2) is 5:1, and 1.5wt% of polyacrylic acid is added.
(2) Mixing the powder with alkali liquor, placing the mixture into a polytetrafluoroethylene lining reaction kettle, placing the reaction kettle into a microwave reactor, setting the reaction temperature to 180 ℃, and reacting for 3 hours.
(3) The supernatant of the lining was poured into a beaker and hydrochloric acid was added dropwise until neutral, and no precipitate was formed.
(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 1h.
2.Na 0.5 K 0.5 Nb 1-y Ta y O 3 Piezoelectric ceramics preparation:
(1) Adding 8% polyvinyl alcohol (PVA) into the powder prepared by a microwave hydrothermal method according to the mass percentage for granulating, prepressing and forming under 50Mpa pressure, and cold isostatic pressing and forming under 200Mpa pressure.
(2) Preserving the temperature at 500 ℃ for 40min to remove PVA, wherein the temperature rising speed is 5 ℃/min.
(3) Plasma spark sintering, axial pressure of 60MPa, sintering temperature of 910 ℃ and sintering time of 5min, annealing treatment in oxygen atmosphere, oxygen flow of 4ml/min, heating speed of 4 ℃/min, heating to 500 ℃, and heat preservation for 4h; oxygen flow rate is 2ml/min, heating speed is 4 ℃/min, heating to 800 ℃, preserving heat for 2.5h, and naturally cooling to room temperature.
(4) The sintered ceramic is subjected to silver plating at 700 ℃ for 0.5h and then polarized, the polarization temperature is 140 ℃, the polarization electric field is 5kv/m, and the polarization time is 25min.
Na prepared in this example 0.5 K 0.5 Nb 0.83 Ta 0.17 O 3 XRD pattern (shown in FIG. 4) and FIG. 1Na 0.5 K 0.5 NbO 3 The main crystal phase in the XRD pattern is consistent.
Example 4:
1.Na 0.5 K 0.5 Nb 0.8 Ta 0.2 O 3 preparing powder:
(1) Adding water into solid KOH and NaOH to prepare mixed alkali liquor with the concentration of 7mol/L, wherein Na + And K + The ratio of Nb is 1:6 respectively 2 O 5 And Ta 2 O 5 The molar ratio of the total added amount of (2) to the alkali liquor is 1:10, wherein Nb 2 O 5 And Ta 2 O 5 The mass molar ratio of (2) was 4:1, and 1.5% by weight of a polycarboxylate ether was added.
(2) Mixing the powder with alkali liquor, placing the mixture into a polytetrafluoroethylene lining reaction kettle, placing the reaction kettle into a microwave reactor, setting the reaction temperature to 170 ℃ and reacting for 4 hours.
(3) The supernatant of the lining was poured into a beaker and hydrochloric acid was added dropwise until neutral, and no precipitate was formed.
(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 1h.
2. Piezoelectric ceramic sample preparation:
(1) Adding 8% polyvinyl alcohol (PVA) into the powder prepared by a microwave hydrothermal method according to the mass percentage for granulating, prepressing and forming under 50Mpa pressure, and cold isostatic pressing and forming under 200Mpa pressure.
(2) Preserving the temperature at 500 ℃ for 40min to remove PVA, wherein the temperature rising speed is 5 ℃/min.
(3) Plasma spark sintering, axial pressure of 60MPa, sintering temperature of 890 ℃, sintering time of 7min, annealing treatment in oxygen atmosphere, oxygen flow of 4ml/min, heating speed of 4 ℃/min, heating to 500 ℃, and preserving heat for 3.5h; oxygen flow rate is 2ml/min, heating speed is 4 ℃/min, heating to 800 ℃, preserving heat for 2.5h, and naturally cooling to room temperature.
(4) The sintered ceramic is subjected to silver plating at 700 ℃ for 0.5h and then polarized, the polarization temperature is 150 ℃, the polarization electric field is 5kv/m, and the polarization time is 25min.
Na prepared in this example 0.5 K 0.5 Nb 0.8 Ta 0.2 O 3 XRD pattern (shown in FIG. 5) and FIG. 1Na 0.5 K 0.5 NbO 3 The main crystal phase in the XRD pattern is consistent.
Comparative example 1: the dispersant of example 1 was removed and the other materials and preparation method were the same as those of example 1.
Comparative example 2: the spark sintering process in example 2 was removed and normal pressure sintering was used, and other materials and preparation methods 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 in example 3.
Comparative example 4: the oxygen flow rates of the first and second temperature rising stages in the annealing process under the oxidizing atmosphere in example 3 were 6ml/min and 2ml/min, respectively, and other raw materials and preparation methods were the same as in example 3.
Comparative example 5: the oxygen flow rates of the first and second temperature rising stages in the annealing process under the oxidizing atmosphere in example 4 were 3ml/min and 1ml/min, respectively, and other raw materials and preparation methods were the same as in example 3.
Comparative example 6: the oxygen flow rates of the first and second temperature rising stages in the annealing process under the oxidizing atmosphere in example 4 were 5ml/min and 3ml/min, respectively, and other raw materials and preparation methods were the same as in example 4.
Comparative example 7: the oxygen flow rates of the first and second temperature rising stages in the annealing process under the oxidizing atmosphere in example 4 were 2ml/min and 3ml/min, respectively, and 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 performance test as shown in table 1 of table 1: performance parameters of piezoelectric ceramics
From the data in table 1, it can be seen that, 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, the relative density of the ceramic matrix sintered at the later stage is low, the compactness is not high, and the performance parameters are reduced. In comparative example 2, normal pressure sintering is adopted, and the ceramic matrix is sintered without spark, so that the relative density is low, the compactness is low, and the performance parameters are reduced. The sintered ceramic matrix in comparative example 3 does not adopt an annealing process under an oxidizing atmosphere, but the density of the ceramic matrix is not much different from that of example 3, but because the sintered ceramic matrix has high oxygen vacancy concentration, the oxygen vacancies have higher migration rate, an internal electric field opposite to the loading electric field is formed under the drive of an external electric field, the internal electric field hinders wall movement, so that the electrical property is poor, the two stages of the annealing process under the oxidizing atmosphere in comparative example 4 adopt 6ml/min and 2ml/min respectively, the performance parameters are worse than those of comparative example 3, the excessive oxygen flow rate can increase new defect distribution, the two stages of the annealing process under the oxidizing atmosphere in comparative example 5 adopt 3ml/min and 1ml/min respectively, and the performance parameters are improved compared with those of comparative example 3, but the level in example 3 is not reached. The comparative example 6 has the same problems as the comparative example 4 in that the oxygen flow rate is excessively large, the piezoelectric ceramic performance is deteriorated, and the piezoelectric ceramic performance in the comparative example 7 is not optimal.
Although the embodiments of the present application have been disclosed in the foregoing description and drawings, it is not limited to the details of the embodiments and examples, but is to be applied to all the fields of application of the present application, it will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the spirit and scope of the application as defined by the appended claims and their equivalents.
Claims (1)
1. A preparation method of Ta-doped potassium-sodium niobate-based piezoelectric ceramic material is characterized in that the general formula of the piezoelectric ceramic material is Na 0.5 K 0.5 Nb 1-y Ta y O 3 Wherein y=0.14;
microwave hydrothermal synthesis of Na 0.5 K 0.5 Nb 1-y Ta y O 3 The preparation method of the powder comprises the following steps:
(1) Adding water into solid NaOH and KOH to prepare mixed alkali liquor with the concentration of 7mol/L as a solvent, wherein Na + And K + The ratio of Nb is 1:6 2 O 5 And Ta 2 O 5 The mass mole of the total amount added and the solventThe molar ratio is 1:8, wherein Nb 2 O 5 And Ta 2 O 5 The mass mol ratio of (2) is 6:1, and 1.5wt% of dispersing agent is added; the dispersing agent is polyacrylic acid;
(2) Mixing and then placing the mixture in a polytetrafluoroethylene lining reaction kettle, placing the reaction kettle in a microwave reactor, setting the reaction temperature to 170 ℃ and the reaction time to 3 hours;
(3) After the reaction is completed, white precipitate is visible at the bottom of the lining, the supernatant of the lining is poured into a beaker, and hydrochloric acid is added dropwise until no precipitate is generated in the neutral state, which indicates that no soluble niobate and tantalate exist in the solution;
(4) Washing the white precipitate at the bottom of the liner to be neutral by deionized water, and drying the white precipitate in an oven at 100 ℃ for 1h;
Na 0.5 K 0.5 Nb 1-y Ta y O 3 the preparation method of the ceramic comprises the following steps:
(1)Na 0.5 K 0.5 Nb 1-y Ta y O 3 washing the powder to an oven for drying, adding 8% polyvinyl alcohol for granulating, prepressing and forming under 40Mpa pressure, and cold isostatic pressing and forming under 210Mpa pressure;
(2) Preserving heat at 500 ℃ for 40min to remove PVA, wherein the temperature rising speed is 5 ℃/min;
(3) Plasma spark sintering, axial pressure of 60MPa, sintering temperature of 890 ℃, sintering time of 5min, annealing treatment in oxygen atmosphere, oxygen flow of 4ml/min, heating speed of 4 ℃/min, heating to 500 ℃, and heat preservation for 3.5h; oxygen flow rate is 2ml/min, heating speed is 4 ℃/min, heating to 800 ℃, preserving heat for 2h, and naturally cooling to room temperature;
(4) The sintered ceramic sample is insulated for 0.5h silver plating polarization at 700 ℃, the polarization temperature is 130 ℃, the polarization electric field is 5kv/m, and the polarization time is 25min.
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| CN116332644B (en) * | 2023-03-17 | 2024-03-22 | 西安建筑科技大学 | K (K) 0.5 Na 0.5 Nb 0.7 Ta 0.3 O 3 Lead-free piezoelectric ceramic material, preparation method and application |
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