CN110981480A - High Tr-tAnd TcLead base of<001>CTextured piezoelectric ceramic material and preparation method thereof - Google Patents

High Tr-tAnd TcLead base of<001>CTextured piezoelectric ceramic material and preparation method thereof Download PDF

Info

Publication number
CN110981480A
CN110981480A CN201910930606.8A CN201910930606A CN110981480A CN 110981480 A CN110981480 A CN 110981480A CN 201910930606 A CN201910930606 A CN 201910930606A CN 110981480 A CN110981480 A CN 110981480A
Authority
CN
China
Prior art keywords
raw materials
psn
ball milling
hours
template
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910930606.8A
Other languages
Chinese (zh)
Inventor
杨帅
李飞
李景雷
周文龙
王领航
刘金凤
徐卓
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian Jiaotong University
Original Assignee
Xian Jiaotong University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian Jiaotong University filed Critical Xian Jiaotong University
Priority to CN201910930606.8A priority Critical patent/CN110981480A/en
Publication of CN110981480A publication Critical patent/CN110981480A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
    • C04B35/497—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates based on solid solutions with lead oxides
    • C04B35/499—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates based on solid solutions with lead oxides containing also titanates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/003—Titanates
    • C01G23/006—Alkaline earth titanates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/442—Carbonates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/95—Products characterised by their size, e.g. microceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention provides a lead base with high Tr-t and Tc<001>C texture piezoelectric ceramic material and preparation method thereof, using (1-x-y) Pb (In)1/2Nb1/2)O3‑xPb(Sc1/2Nb1/2)O3‑yPbTiO3The (PIN-PSN-PT) system is used as the texture ceramic powder, x and y both represent mole fractions, x is more than or equal to 0.405 and less than or equal to 0.445, and y is more than or equal to 0.365 and less than or equal to 0.405; in that<001>CThe BT template is textured, and the main principle is that PIN-PSN-PT ceramic powder is horizontal<001>CCarrying out directional growth on a BT template to obtain an anisotropic structure similar to a single crystal, thereby obtaining piezoelectric performance close to the single crystal, combining with polarization of a 4R engineering domain in a non-spontaneous polarization direction on the basis, and finally obtaining the high-voltage crystalTr‑tAnd TcAnd textured ceramics with higher piezoelectric performance.

Description

High Tr-tAnd TcLead radical of (001)CTextured piezoelectric ceramicsCeramic material and preparation method thereof
Technical Field
The invention belongs to the technical field of piezoelectric ceramic materials, and particularly relates to a high Tr-tAnd TcLead base of<001>CA textured piezoelectric ceramic material and a preparation method thereof.
Background
Piezoelectric materials are materials that produce a potential difference in the direction of polarity when an external stress is applied, whereas a mechanical strain is produced when an electric field is applied (the direction of strain depends on the polarization of the material and the orientation of the potential difference). Due to this physical property, piezoelectric materials are widely used in hydrophones, transducers, sensors, energy collectors, and the like. The related piezoelectric devices and products are developing towards miniaturization, light weight, high power and multiple functions, which puts higher requirements on the piezoelectric coefficient, the electromechanical coupling coefficient and the thermal stability of the piezoelectric material.
Common piezoelectric ceramics, single crystals and textured ceramics are three typical piezoelectric materials, and for the piezoelectric properties of materials with the same components, the common piezoelectric ceramics are far lower than the piezoelectric single crystals, and the textured ceramics are between the common piezoelectric ceramics and the single crystals, the better the quality of the textured ceramics is, and the closer the piezoelectric properties are to the single crystals; for production cost, the single crystal is generally grown by a melting method, for example: bridgman; therefore, the method has bright prospect of replacing single crystals by using the low-cost high-performance textured ceramics.
The existing piezoelectric ceramics comprise two types of lead-free piezoelectric ceramics and lead-based piezoelectric ceramics system, which are distinguished by lead element, and the performance of the lead-based ceramics is generally much higher than that of the lead-free ceramics, although the lead-free piezoelectric ceramics have been reported to have similar individual performance to the lead-based ceramics in recent years, for example: piezoelectric coefficient (d)33) Curie temperature (T)c) However, the phase transition temperature, the electromechanical coupling coefficient and the coercive field of the lead-based ceramic are far lower than those of lead-based ceramic, and the requirements of practical application are far from being met.
The lead-based textured piezoelectric ceramic is mainly divided into (1-x) Pb(Mg1/3Nb2/3)O3-xPbTiO3(PMN-PT) with (1-x-y) Pb (In)1/2Nb1/2)O3-xPb(Mg1/3Nb2/3)O3-yPbTiO3(PIN-PMN-PT) two types, wherein PMN-PT textured ceramics have d33The temperature is 500-1200pC/N, the Curie temperature is lower than 170 ℃, the phase transition temperature is lower than 100 ℃, and when the temperature is higher than the phase transition temperature, the performance of the piezoelectric material greatly slides down, so that the application of the piezoelectric material in a device is limited by the life defect; d of PIN-PMN-PT textured ceramic33Is 780-doped 920pC/N, the Curie temperature is lower than 220 ℃, the phase transition temperature is lower than 120 ℃, and the phase transition temperature is improved to a certain extent compared with a PMN-PT system, but the requirements of an ultrasonic device can not be met, and needs to be further improved.
Disclosure of Invention
The invention provides a high Tr-tAnd TcLead base of<001>CThe textured piezoelectric ceramic material and the preparation method thereof solve the problem that the lead-based textured piezoelectric ceramic in the prior art cannot meet the requirements of ultrasonic devices.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides perovskite phase PIN-PSN-PT powder which comprises three-phase solid solution, wherein the first phase is Pb (In)1/2Nb1/2)O3The second phase is Pb (Sc)1/2Nb1/2)O3The third phase is PbTiO3The chemical formula is (1-x-y) Pb (In)1/ 2Nb1/2)O3–xPb(Sc1/2Nb1/2)O–y PbTiO3Wherein x and y both represent mole fractions, x is more than or equal to 0.405 and less than or equal to 0.445, and y is more than or equal to 0.365 and less than or equal to 0.405.
A preparation method of perovskite phase PIN-PSN-PT powder comprises the following steps:
according to (1-x-y) Pb (In)1/2Nb1/2)O3–xPb(Sc1/2Nb1/2)O–y PbTiO3(PIN-PSN-PT) in a stoichiometric ratio, ball milling with absolute ethyl alcohol as a medium, drying, presintering, and finally obtaining perovskite phase PIN-PSN-PT powder.
Preferably, the process conditions of the pre-firing are: presintering at 750-900 deg.c for 2 hr.
High Tr-tAnd TcLead base of<001>CThe preparation method of the textured piezoelectric ceramic material comprises the following steps:
s1, preparation<001>CBaTiO3A template;
s2, transformation of the DNA fragment obtained in S1<001>CBaTiO3Adding fluxing agent, dispersing agent, adhesive, plasticizer, solvent and perovskite phase PIN-PSN-PT powder into the template, uniformly mixing, and performing ball milling to finally obtain slurry, wherein the fluxing agent, the solvent and the perovskite phase PIN-PSN-PT powder are mixed<001>CBaTiO3The mass ratio of the template is (0.125-2): 1; dispersing agent, adhesive, plasticizer, solvent and perovskite phase PIN-PSN-PT powder<001>CBaTiO3The volume ratio of the template is (1.5-3.5): (4-6.5): (4-7): (50-70): (3-7);
s3, removing bubbles from the slurry obtained in the S2, and then carrying out tape casting to obtain a film;
s4, sequentially cutting, laminating and hot-press forming the film obtained in the S3 to obtain a ceramic green body;
s5, carrying out degumming on the ceramic green body obtained in the S4, and then carrying out cold isostatic pressing treatment to obtain a compact ceramic green body;
s6, sintering the compact ceramic blank obtained in the S5 to finally obtain the high Tr-tAnd TcLead base of<001>CTextured piezoceramic materials.
Preferably, in S1, preparation<001>CBaTiO3The specific method of the template is as follows:
prepared by adopting a two-step topological chemical method<001>CBaTiO3Template, reaction equation is as follows:
2Bi2O3+3TiO2→Bi4Ti3O12
Bi4Ti3O12+3BaCO3→3BaTiO3
first, Bi is weighed in a stoichiometric ratio2O3And TiO2Then adding Bi2O3And TiO2The mixture is uniformly mixed with KCl according to the mass ratio of 1: 1; then carrying out molten salt reaction to prepare Bi4Ti3O12；
Next, Bi was weighed in a stoichiometric ratio4Ti3O12And BaCO3Then adding Bi4Ti3O12And BaCO3With KCl according to 1: 1.5, uniformly mixing; then carrying out molten salt reaction, and finally washing and pickling to obtain the product<001>CBaTiO3And (5) template.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a lead base with high Tr-t and Tc<001>C texture piezoelectric ceramic material and preparation method thereof, using (1-x-y) Pb (In)1/2Nb1/2)O3-xPb(Sc1/2Nb1/2)O3-yPbTiO3The (PIN-PSN-PT) system is used as the texture ceramic powder, x and y both represent mole fractions, x is more than or equal to 0.405 and less than or equal to 0.445, and y is more than or equal to 0.365 and less than or equal to 0.405; in that<001>CThe BT template is textured, and the main principle is that PIN-PSN-PT ceramic powder is horizontal<001>CCarrying out directional growth on a BT template to obtain an anisotropic structure similar to a single crystal, thereby obtaining piezoelectric performance close to the single crystal, combining with polarization of a 4R engineering domain in a non-spontaneous polarization direction on the basis, and finally obtaining the high Tr-tAnd TcAnd textured ceramics with higher piezoelectric performance.
The texture degree, the piezoelectric coefficient, the Curie temperature and the coercive field of the textured ceramic based on the PIN-PSN-PT system are respectively 97.2 percent, 792pC/N, 262 ℃ and 6.8kV/cm, wherein the piezoelectric coefficient is 2.78 times of that of common ceramic, and the textured ceramic shows good temperature stability within the range of 25-200 ℃, the piezoelectric coefficient is only reduced by 10 percent, and the electromechanical coupling coefficient k is33The content was 84%. The characteristics show that the textured ceramic of the PIN-PSN-PT system is expected to be widely applied in the fields of ultrasonic transducers, hydrophones and the like.
Drawings
FIG. 1: the X-ray diffraction pattern of the ceramic material of the invention.
FIG. 2 is a drawing: the invention discloses a scanning electron microscope atlas of a ceramic material.
FIG. 3: the dielectric constant and the dielectric loss of the ceramic material change with temperature.
FIG. 4 is a drawing: the electrostrictive pattern of the ceramic material of the present invention.
FIG. 5: the piezoelectric coefficient and the dielectric property of the ceramic material are compared with those of common ceramics.
Detailed Description
The present invention will be described in further detail with reference to examples.
A perovskite phase PIN-PSN-PT powder comprises a three-phase solid solution, and a first phase is Pb (In)1/2Nb1/2)O3The second phase is Pb (Sc)1/2Nb1/2)O3The third phase is PbTiO3The chemical formula is (1-x-y) Pb (In)1/2Nb1/2)O3–xPb(Sc1/2Nb1/2)O–y PbTiO3Wherein x and y both represent mole fractions, x is more than or equal to 0.405 and less than or equal to 0.445, and y is more than or equal to 0.365 and less than or equal to 0.405.
According to (1-x-y) Pb (In)1/2Nb1/2)O3–xPb(Sc1/2Nb1/2)O–y PbTiO3(PIN-PSN-PT) in a stoichiometric ratio, ball milling with absolute ethyl alcohol as a medium, drying, and presintering at the temperature of 750-.
High Tr-tAnd TcLead base of<001>CThe preparation method of the textured piezoelectric ceramic material comprises the following steps:
s1, preparation<001>CBaTiO3A template;
s2, transformation of the DNA fragment obtained in S1<001>CBaTiO3Adding fluxing agent, dispersing agent, adhesive, plasticizer, solvent and perovskite phase PIN-PSN-PT powder into the template, uniformly mixing, and performing ball milling to finally obtain slurry, wherein the fluxing agent, the solvent and the perovskite phase PIN-PSN-PT powder are mixed<001>CBaTiO3Of moulding boardsThe mass ratio is (0.125-2%): 1; dispersing agent, adhesive, plasticizer, solvent and perovskite phase PIN-PSN-PT powder<001>CBaTiO3The volume ratio of the template is 1.5-3.5%, 4-6.5%, 4-7%, 50-70% and 3-7%
S3, removing bubbles from the slurry obtained in the S2, and then carrying out tape casting to obtain a film;
s4, sequentially cutting, laminating and hot-press forming the film obtained in the S3 to obtain a ceramic green body;
s5, carrying out degumming on the ceramic green body obtained in the S4, and then carrying out cold isostatic pressing treatment to obtain a compact ceramic green body;
s6, sintering the compact ceramic blank obtained in the S5 to finally obtain the high Tr-tAnd TcLead base of<001>CTextured piezoceramic materials.
Wherein, in S1, preparation<001>CBaTiO3The specific method of the template is as follows:
prepared by adopting a two-step topological chemical method<001>CBaTiO3Template, reaction equation is as follows:
2Bi2O3+3TiO2→Bi4Ti3O12
Bi4Ti3O12+3BaCO3→3BaTiO3
first, Bi is weighed in a stoichiometric ratio2O3And TiO2Then adding Bi2O3And TiO2The mixture is uniformly mixed with KCl according to the mass ratio of 1: 1; then carrying out molten salt reaction to prepare Bi4Ti3O12；
Next, Bi was weighed in a stoichiometric ratio4Ti3O12And BaCO3Then adding Bi4Ti3O12And BaCO3With KCl according to 1: 1.5, uniformly mixing; then carrying out molten salt reaction, and finally washing and pickling to obtain the product<001>CBaTiO3And (5) template.
Example 1
(1) Bi with the purity of 99.99 percent is adopted2O3，99.99％TiO2And 99.99% KCl as raw materials, respectively weighing 140.21, 36.12 and 176.33 g, and then putting the raw materials into a ball milling tank for ball milling and mixing, wherein the volume of the raw materials is as follows: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is equal to 1: 2: 4, ball-milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at 120 ℃; after drying, keeping the temperature at 1100 ℃ for 6 hours; washing with hot deionized water for multiple times to obtain pure layered Bi4Ti3O12。
(2) Adopting the precursor powder Bi in the step (1)4Ti3O12BaCO with purity of 99.99%3And 99.99% KCl as raw materials, respectively weighing 29.29, 49.36 and 94.35 g, and then putting into a ball milling tank for ball milling and mixing, wherein the volume of the raw materials is as follows: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is equal to 1: 2: and 4, ball milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at the temperature of 120 ℃. After drying, keeping the temperature at 1020 ℃ for 3 hours; washing with hot deionized water, adding 3mol/L nitric acid solution for acid washing, washing with hot deionized water for several times, and drying to obtain the final product<001>CBaTiO3。
(3) In with a purity of 99.99% was used2O3And 99.99% Nb2O5Weighing 30.66 and 29.34 of raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials at 1100 ℃ for 2 hours to synthesize InNbO4(IN); sc with the purity of 99.99 percent is adopted2O3And 99.99% Nb2O5Weighing 20.63 and 39.36 of raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing, carrying out ball milling for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials at 1200 ℃ for 2 hours to synthesize ScNbO4(SN)。
(4) Using IN and SN obtained IN the step (3) and Pb with the purity of 98 percent3O4And TiO with a purity of 99.99%2Weighing 7.84, 13.67, 69.61 and 8.87 serving as raw materials respectivelyAnd g, putting the mixture into a ball milling pot, ball milling and mixing the mixture for 12 hours, drying the mixture, and then preserving the heat at 850 ℃ for 2 hours to synthesize pure PIN-xPSN-yPT ceramic powder, wherein x and y represent mole numbers, x is 0.445, and y is 0.365.
(5) Weighing 30g of PIN-PSN-PT ceramic powder synthesized in the step (4), and gradually adding CuO, ethanol, xylene, KD-1, polyvinyl butyral (PVB), phthalate (BBP), polyethylene glycol (PAG) and<001>CBaTiO3templates, having masses of 0.075, 1.2, 0.49, 0.6, 0.45 and 1.5g, were ball milled for a total of 48 hours to obtain a slurry.
(6) And (3) defoaming the slurry obtained in the step (5), then carrying out tape casting, wherein the tape casting speed of a scraper is 8cm/min, the thickness between the tape casting scraper and a bottom film is 200 mu m, drying at room temperature for 8 hours after tape casting, and cutting the film into a square with the side length of 30mm by using a blade.
(7) And (4) laminating the square membrane obtained in the step (6), hot-pressing for 15min at the pressure of 15MPa and the temperature of 70 ℃, and then cutting the lamination into square biscuit bodies with uniform size by a blade.
(8) And (4) preserving the heat of the biscuit obtained in the step (7) for 2h at 600 ℃ for glue discharging, and then maintaining the pressure of the biscuit in a cold isostatic press at 200MPa for 10min to obtain the biscuit with high density.
(9) And (3) preserving the biscuit obtained in the step (8) at 1100-1250 ℃ for 10 hours to obtain a final ceramic sample.
(10) And (4) polishing smooth and parallel thin slices with the thickness of about 0.5mm on two surfaces of the ceramic sample obtained in the step (9), and testing the polished ceramic sample after being coated with a silver electrode.
Example 2
(1) Bi with the purity of 99.99 percent is adopted2O3，99.99％TiO2And 99.99% KCl as raw materials, respectively weighing 140.21, 36.12 and 176.33 g, and then putting the raw materials into a ball milling tank for ball milling and mixing, wherein the volume of the raw materials is as follows: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is equal to 1: 2: 4, ball-milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at 120 ℃; after drying, keeping the temperature at 1100 ℃ for 6 hours; washing with hot deionized water for multiple times to obtain pure layered Bi4Ti3O12。
(2) Adopting the precursor powder Bi in the step (1)4Ti3O12BaCO with purity of 99.99%3And 99.99% KCl as raw materials, respectively weighing 29.29, 49.36 and 94.35 g, and then putting into a ball milling tank for ball milling and mixing, wherein the volume of the raw materials is as follows: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is equal to 1: 2: and 4, ball milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at the temperature of 120 ℃. After drying, keeping the temperature at 1020 ℃ for 3 hours; washing with hot deionized water, adding 3mol/L nitric acid solution for acid washing, washing with hot deionized water for several times, and drying to obtain the final product<001>CBaTiO3。
(3) In with a purity of 99.99% was used2O3And 99.99% Nb2O5Weighing 30.66 and 29.34 of raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials at 1100 ℃ for 2 hours to synthesize InNbO4(IN); sc with the purity of 99.99 percent is adopted2O3And 99.99% Nb2O5Weighing 20.63 and 39.36 of raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing, carrying out ball milling for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials at 1200 ℃ for 2 hours to synthesize ScNbO4(SN)。
(4) Using IN and SN obtained IN the step (3) and Pb with the purity of 98 percent3O4And TiO with a purity of 99.99%2Weighing 7.84, 13.06, 69.61 and 9.36 g of raw materials respectively, then putting the raw materials into a ball milling pot for ball milling and mixing for 12 hours, drying the raw materials, and then preserving the heat at 850 ℃ for 2 hours to synthesize pure PIN-xPSN-yPT ceramic powder, wherein x and y represent mole numbers, x is 0.425, and y is 0.385.
(5) Weighing 30g of PIN-PSN-PT ceramic powder synthesized in the step (4), and gradually adding CuO, ethanol, xylene, KD-1, polyvinyl butyral (PVB), phthalate (BBP), polyethylene glycol (PAG) and<001>CBaTiO3templates with masses of 0.075, 1.2, 0.49, 0.6, 0.45 and 1, respectively.5g, and a total of 48 hours of ball milling to obtain a slurry.
(6) And (3) defoaming the slurry obtained in the step (5), then carrying out tape casting, wherein the tape casting speed of a scraper is 8cm/min, the thickness between the tape casting scraper and a bottom film is 200 mu m, drying at room temperature for 8 hours after tape casting, and cutting the film into a square with the side length of 30mm by using a blade.
(7) And (4) laminating the square membrane obtained in the step (6), hot-pressing for 15min at the pressure of 15MPa and the temperature of 70 ℃, and then cutting the lamination into square biscuit bodies with uniform size by a blade.
(8) And (4) preserving the heat of the biscuit obtained in the step (7) for 2h at 600 ℃ for glue discharging, and then maintaining the pressure of the biscuit in a cold isostatic press at 200MPa for 10min to obtain the biscuit with high density.
(9) And (3) preserving the biscuit obtained in the step (8) at 1100-1250 ℃ for 10 hours to obtain a final ceramic sample.
(10) And (4) polishing smooth and parallel thin slices with the thickness of about 0.5mm on two surfaces of the ceramic sample obtained in the step (9), and testing the polished ceramic sample after being coated with a silver electrode.
Example 3
(1) Bi with the purity of 99.99 percent is adopted2O3，99.99％TiO2And 99.99% KCl as raw materials, respectively weighing 140.21, 36.12 and 176.33 g, and then putting the raw materials into a ball milling tank for ball milling and mixing, wherein the volume of the raw materials is as follows: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is equal to 1: 2: 4, ball-milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at 120 ℃; after drying, keeping the temperature at 1100 ℃ for 6 hours; washing with hot deionized water for multiple times to obtain pure layered Bi4Ti3O12。
(2) Adopting the precursor powder Bi in the step (1)4Ti3O12BaCO3 with the purity of 99.99% and KCl with the purity of 99.99% are taken as raw materials, 29.29 g, 49.36 g and 94.35 g are respectively weighed and then put into a ball milling tank for ball milling and mixing, and the volume of the raw materials is as follows during ball milling: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is equal to 1: 2: and 4, ball milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at the temperature of 120 ℃. After drying, keeping the temperature at 1020 ℃ for 3 hours; by usingThe salt is washed clean by hot deionized water, then 3mol/L nitric acid solution is added for acid washing, then the hot deionized water is used for water washing for a plurality of times, and then the mixture is dried to obtain the product<001>CBaTiO3。
(3) In with a purity of 99.99% was used2O3And 99.99% Nb2O5Weighing 30.66 and 29.34 of raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials at 1100 ℃ for 2 hours to synthesize InNbO4(IN); sc with the purity of 99.99 percent is adopted2O3And 99.99% Nb2O5Weighing 20.63 and 39.36 of raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing, carrying out ball milling for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials at 1200 ℃ for 2 hours to synthesize ScNbO4(SN)。
(4) Using IN and SN obtained IN the step (3) and Pb with the purity of 98 percent3O4And TiO with a purity of 99.99%2Weighing 7.84, 12.45, 69.61 and 9.85 g of the raw materials respectively, then putting the raw materials into a ball milling pot for ball milling and mixing for 12 hours, drying the raw materials, and then preserving the heat at 850 ℃ for 2 hours to synthesize pure PIN-xPSN-yPT ceramic powder, wherein x and y represent mole numbers, x is 0.405, and y is 0.405.
(5) Weighing 30g of PIN-PSN-PT ceramic powder synthesized in the step (4), and gradually adding CuO, ethanol, xylene, KD-1, polyvinyl butyral (PVB), phthalate (BBP), polyethylene glycol (PAG) and<001>CBaTiO3templates, having masses of 0.075, 1.2, 0.49, 0.6, 0.45 and 1.5g, were ball milled for a total of 48 hours to obtain a slurry.
(6) And (3) defoaming the slurry obtained in the step (5), then carrying out tape casting, wherein the tape casting speed of a scraper is 8cm/min, the thickness between the tape casting scraper and a bottom film is 200 mu m, drying at room temperature for 8 hours after tape casting, and cutting the film into a square with the side length of 30mm by using a blade.
(7) And (4) laminating the square membrane obtained in the step (6), hot-pressing for 15min at the pressure of 15MPa and the temperature of 70 ℃, and then cutting the lamination into square biscuit bodies with uniform size by a blade.
(8) And (4) preserving the heat of the biscuit obtained in the step (7) for 2h at 600 ℃ for glue discharging, and then maintaining the pressure of the biscuit in a cold isostatic press at 200MPa for 10min to obtain the biscuit with high density.
(9) And (3) preserving the biscuit obtained in the step (8) at 1100-1250 ℃ for 10 hours to obtain a final ceramic sample.
(10) And (4) polishing smooth and parallel thin slices with the thickness of about 0.5mm on two surfaces of the ceramic sample obtained in the step (9), and testing the polished ceramic sample after being coated with a silver electrode.
Example 4
(1) Bi with the purity of 99.99 percent is adopted2O3，99.99％TiO2And 99.99% KCl as raw materials, respectively weighing 140.21, 36.12 and 176.33 g, and then putting the raw materials into a ball milling tank for ball milling and mixing, wherein the volume of the raw materials is as follows: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is approximately equal to 1: 2: 4, ball milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at 120 ℃; after drying, keeping the temperature at 1100 ℃ for 6 hours; washing with hot deionized water for multiple times to obtain pure layered Bi4Ti3O12。
(2) Adopting the precursor powder Bi in the step (1)4Ti3O12BaCO with purity of 99.99%3And 99.99% KCl as raw materials, respectively weighing 29.29, 49.36 and 94.35 g, and then putting into a ball milling tank for ball milling and mixing, wherein the volume of the raw materials is as follows: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is approximately equal to 1: 2: 4 ball milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at 120 ℃. After drying, keeping the temperature at 1020 ℃ for 3 hours; washing with hot deionized water, adding 3mol/L nitric acid solution for acid washing, washing with hot deionized water for several times, and drying to obtain the final product<001>CBaTiO3。
(3) In with a purity of 99.99% was used2O3And 99.99% Nb2O5Weighing 30.66 and 29.34 of the raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials for 2 hours at 1100 ℃ to obtain the productInto InNbO4(IN); sc with the purity of 99.99 percent is adopted2O3And 99.99% Nb2O5Weighing 20.63 and 39.36 of raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing, carrying out ball milling for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials at 1200 ℃ for 2 hours to synthesize ScNbO4(SN)。
(4) Using IN and SN obtained IN the step (3), Pb3O4 with the purity of 98 percent and TiO with the purity of 99.99 percent2Weighing 7.84, 13.67, 69.61 and 8.87 g of raw materials respectively, then putting the raw materials into a ball milling pot for ball milling and mixing for 12 hours, drying the raw materials, and then preserving the heat at 850 ℃ for 2 hours to synthesize pure PIN-xPSN-yPT ceramic powder, wherein x and y represent mole numbers, x is 0.445, and y is 0.365.
(5) Weighing 30g of PIN-PSN-PT ceramic powder synthesized in the step (4), and gradually adding B2O3Ethanol, xylene, KD-1, polyvinyl butyral (PVB), phthalate (BBP), polyethylene glycol (PAG) and<001>CBaTiO3templates, having masses of 0.3, 1.2, 0.49, 0.6, 0.45 and 1.5g, were ball-milled for a total of 48 hours to obtain a slurry.
(6) And (3) defoaming the slurry obtained in the step (5), then carrying out tape casting, wherein the tape casting speed of a scraper is 8cm/min, the thickness between the tape casting scraper and a bottom film is 200 mu m, drying at room temperature for 8 hours after tape casting, and cutting the film into a square with the side length of 30mm by using a blade.
(7) And (4) laminating the square membrane obtained in the step (6), hot-pressing for 15min at the pressure of 15MPa and the temperature of 70 ℃, and then cutting the lamination into square biscuit bodies with uniform size by a blade.
(8) And (4) preserving the heat of the biscuit obtained in the step (7) for 2h at 600 ℃ for glue discharging, and then maintaining the pressure of the biscuit in a cold isostatic press at 00MPa for 10min to obtain the biscuit with high density.
(9) And (3) preserving the biscuit obtained in the step (8) at 1100-1250 ℃ for 10 hours to obtain a final ceramic sample.
(10) And (4) polishing smooth and parallel thin slices with the thickness of about 0.5mm on two surfaces of the ceramic sample obtained in the step (9), and testing the polished ceramic sample after being coated with a silver electrode.
Example 5
(1) Bi2O3 with the purity of 99.99 percent and TiO with the purity of 99.99 percent are adopted2And 99.99% KCl as raw materials, respectively weighing 140.21, 36.12 and 176.33 g, and then putting the raw materials into a ball milling tank for ball milling and mixing, wherein the volume of the raw materials is as follows: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is approximately equal to 1: 2: 4, ball milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at 120 ℃; after drying, keeping the temperature at 1100 ℃ for 6 hours; washing with hot deionized water for multiple times to obtain pure layered Bi4Ti3O12。
(2) Adopting the precursor powder Bi in the step (1)4Ti3O12BaCO with purity of 99.99%3And 99.99% KCl as raw materials, respectively weighing 29.29, 49.36 and 94.35 g, and then putting into a ball milling tank for ball milling and mixing, wherein the volume of the raw materials is as follows: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is approximately equal to 1: 2: 4 ball milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at 120 ℃. After drying, keeping the temperature at 1020 ℃ for 3 hours; washing with hot deionized water, adding 3mol/L nitric acid solution for acid washing, washing with hot deionized water for several times, and drying to obtain the final product<001>CBaTiO3。
(3) In with a purity of 99.99% was used2O3And 99.99% Nb2O5Weighing 30.66 and 29.34 of raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials at 1100 ℃ for 2 hours to synthesize InNbO4(IN); sc with the purity of 99.99 percent is adopted2O3And 99.99% Nb2O5Weighing 20.63 and 39.36 of raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing, carrying out ball milling for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials at 1200 ℃ for 2 hours to synthesize ScNbO4(SN)。
(4) Using IN and SN obtained IN the step (3) and Pb with the purity of 98 percent3O4And TiO with a purity of 99.99%2Weighing 7.84, 13.06, 69.61 and 9.36 g of the raw materials respectivelyAnd then putting the mixture into a ball milling pot for ball milling and mixing for 12 hours, drying the mixture, and then preserving the heat for 2 hours at 850 ℃ to synthesize pure PIN-xPSN-yPT ceramic powder, wherein x and y represent mole numbers, x is 0.425, and y is 0.385.
(5) Weighing 30g of PIN-PSN-PT ceramic powder synthesized in the step (4), and gradually adding B2O3Ethanol, xylene, KD-1, polyvinyl butyral (PVB), phthalate (BBP), polyethylene glycol (PAG) and<001>CBaTiO3templates, having masses of 0.3, 1.2, 0.49, 0.6, 0.45 and 1.5g, were ball-milled for a total of 48 hours to obtain a slurry.
(6) And (3) defoaming the slurry obtained in the step (5), then carrying out tape casting, wherein the tape casting speed of a scraper is 8cm/min, the thickness between the tape casting scraper and a bottom film is 200 mu m, drying at room temperature for 8 hours after tape casting, and cutting the film into a square with the side length of 30mm by using a blade.
(7) And (4) laminating the square membrane obtained in the step (6), hot-pressing for 15min at the pressure of 15MPa and the temperature of 70 ℃, and then cutting the lamination into square biscuit bodies with uniform size by a blade.
(8) And (4) preserving the heat of the biscuit obtained in the step (7) for 2h at 600 ℃ for glue discharging, and then maintaining the pressure of the biscuit in a cold isostatic press at 00MPa for 10min to obtain the biscuit with high density.
(9) And (3) preserving the biscuit obtained in the step (8) at 1100-1250 ℃ for 10 hours to obtain a final ceramic sample.
(10) And (4) polishing smooth and parallel thin slices with the thickness of about 0.5mm on two surfaces of the ceramic sample obtained in the step (9), and testing the polished ceramic sample after being coated with a silver electrode.
Example 6
(1) Bi with the purity of 99.99 percent is adopted2O3，99.99％TiO2And 99.99% KCl as raw materials, respectively weighing 140.21, 36.12 and 176.33 g, and then putting the raw materials into a ball milling tank for ball milling and mixing, wherein the volume of the raw materials is as follows: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is approximately equal to 1: 2: 4, ball milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at 120 ℃; after drying, keeping the temperature at 1100 ℃ for 6 hours; washing with hot deionized water for several times to obtain pure productLayered Bi of4Ti3O12。
(2) Adopting the precursor powder Bi in the step (1)4Ti3O12BaCO with purity of 99.99%3And 99.99% KCl as raw materials, respectively weighing 29.29, 49.36 and 94.35 g, and then putting into a ball milling tank for ball milling and mixing, wherein the volume of the raw materials is as follows: agate sphere volume: the volume ratio of the ball milling meson absolute ethyl alcohol is approximately equal to 1: 2: 4 ball milling for 12 hours, and then putting the ball-milled raw materials into an oven to be dried for 5 hours at 120 ℃. After drying, keeping the temperature at 1020 ℃ for 3 hours; washing with hot deionized water, adding 3mol/L nitric acid solution for acid washing, washing with hot deionized water for several times, and drying to obtain the final product<001>CBaTiO3。
(3) In with a purity of 99.99% was used2O3And 99.99% Nb2O5Weighing 30.66 and 29.34 of raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials at 1100 ℃ for 2 hours to synthesize InNbO4(IN); sc with the purity of 99.99 percent is adopted2O3And 99.99% Nb2O5Weighing 20.63 and 39.36 of raw materials respectively, then putting the raw materials into a ball milling tank for ball milling and mixing, carrying out ball milling for 12 hours, finally drying the raw materials in an oven, and preserving the heat of the dried raw materials at 1200 ℃ for 2 hours to synthesize ScNbO4(SN)。
(4) Using IN and SN obtained IN the step (3), Pb3O4 with the purity of 98 percent and TiO with the purity of 99.99 percent2Weighing 7.84, 12.45, 69.61 and 9.85 g of the raw materials respectively, then putting the raw materials into a ball milling pot for ball milling and mixing for 12 hours, drying the raw materials, and then preserving the heat at 850 ℃ for 2 hours to synthesize pure PIN-xPSN-yPT ceramic powder, wherein x and y represent mole numbers, x is 0.405, and y is 0.405.
(5) Weighing 30g of PIN-PSN-PT ceramic powder synthesized in the step (4), and gradually adding B2O3Ethanol, xylene, KD-1, polyvinyl butyral (PVB), phthalate (BBP), polyethylene glycol (PAG) and<001>CBaTiO3the mass of the template is 0.3, 1.2, 0.49, 0.6 and 0 respectively.45. 0.45 and 1.5g, obtained after a total of 48 hours of ball milling.
(6) And (3) defoaming the slurry obtained in the step (5), then carrying out tape casting, wherein the tape casting speed of a scraper is 8cm/min, the thickness between the tape casting scraper and a bottom film is 200 mu m, drying at room temperature for 8 hours after tape casting, and cutting the film into a square with the side length of 30mm by using a blade.
(7) And (4) laminating the square membrane obtained in the step (6), hot-pressing for 15min at the pressure of 15MPa and the temperature of 70 ℃, and then cutting the lamination into square biscuit bodies with uniform size by a blade.
(8) And (4) preserving the heat of the biscuit obtained in the step (7) for 2h at 600 ℃ for glue discharging, and then maintaining the pressure of the biscuit in a cold isostatic press at 00MPa for 10min to obtain the biscuit with high density.
(9) And (3) preserving the biscuit obtained in the step (8) at 1100-1250 ℃ for 10 hours to obtain a final ceramic sample.
(10) And (4) polishing smooth and parallel thin slices with the thickness of about 0.5mm on two surfaces of the ceramic sample obtained in the step (9), and testing the polished ceramic sample after being coated with a silver electrode.
The phase structure of the ceramic was prepared by X-ray diffraction measurements, as shown in figure 1; it can be seen from the figure that a certain amount of B is added2O3Or after CuO, the texture degree (F) can be greatly improved(001)>96%) indicating a ceramic rim<001>Degree of directionally oriented growth.
As can be seen from FIG. 2, the PIN-PSN-PT ceramic powder is formed along<001>CThe BT template (the crystal grains of the slender strip) is directionally grown, and the size of the crystal grains is 15-35 mu m.
From FIG. 3, the dielectric constant and dielectric loss are shown as a function of temperature, and T of the textured PIN-PSN-PT ceramic can be showncThe temperature is reduced by 5-10 ℃ and the temperature stability is almost unchanged.
It can be seen from FIG. 4 that the strain coefficient of the textured PIN-PSN-PT ceramic is more than 2 times that of the ordinary PIN-PSN-PT ceramic.
The piezoelectric coefficient (d) of the textured PIN-PSN-PT ceramic can be seen in FIG. 533) Compared with the common ceramic, the ceramic is improved from 285pC/N to 792pC/N, which is 2.78 times that of the common ceramic; dielectric constant is increased from 997 to 1900。

Claims (5)

1. A perovskite phase PIN-PSN-PT powder, characterized In that the composition comprises a three-phase solid solution, the first phase being Pb (In)1/2Nb1/2)O3The second phase is Pb (Sc)1/2Nb1/2)O3The third phase is PbTiO3The chemical formula is (1-x-y) Pb (In)1/ 2Nb1/2)O3–xPb(Sc1/2Nb1/2)O–y PbTiO3Wherein x and y both represent mole fractions, x is more than or equal to 0.405 and less than or equal to 0.445, and y is more than or equal to 0.365 and less than or equal to 0.405.
2. A preparation method of perovskite phase PIN-PSN-PT powder is characterized by comprising the following steps:
according to (1-x-y) Pb (In)1/2Nb1/2)O3–xPb(Sc1/2Nb1/2)O–y PbTiO3(PIN-PSN-PT) in a stoichiometric ratio, ball milling with absolute ethyl alcohol as a medium, drying, presintering, and finally obtaining perovskite phase PIN-PSN-PT powder.
3. The method for preparing perovskite phase PIN-PSN-PT powder according to claim 2, characterized in that the presintering process conditions are as follows: presintering at 750-900 deg.c for 2 hr.
4. High Tr-tAnd TcLead base of<001>CThe preparation method of the textured piezoelectric ceramic material is characterized by comprising the following steps of:
s1, preparation<001>CBaTiO3A template;
s2, transformation of the DNA fragment obtained in S1<001>CBaTiO3Adding fluxing agent, dispersing agent, adhesive, plasticizer, solvent and perovskite phase PIN-PSN-PT powder into the template, uniformly mixing, and performing ball milling to finally obtain slurry, wherein the fluxing agent, the solvent and the perovskite phase PIN-PSN-PT powder are mixed<001>CBaTiO3The mass ratio of the template is (0.125-2%): 1; dispersant, binder, plasticizer, solvent and perovskiteThe respective phase PIN-PSN-PT powder<001>CBaTiO3The volume ratio of the template is 1.5-3.5%, 4-6.5%, 4-7%, 50-70% and 3-7%
S3, removing bubbles from the slurry obtained in the S2, and then carrying out tape casting to obtain a film;
s4, sequentially cutting, laminating and hot-press forming the film obtained in the S3 to obtain a ceramic green body;
s5, carrying out degumming on the ceramic green body obtained in the S4, and then carrying out cold isostatic pressing treatment to obtain a compact ceramic green body;
s6, sintering the compact ceramic blank obtained in the S5 to finally obtain the high Tr-tAnd TcLead base of<001>CTextured piezoceramic materials.
5. A high T according to claim 4r-tAnd TcLead base of<001>CThe preparation method of the textured piezoelectric ceramic material is characterized by preparing in S1<001>CBaTiO3The specific method of the template is as follows:
prepared by adopting a two-step topological chemical method<001>CBaTiO3Template, reaction equation is as follows:
2Bi2O3+3TiO2→Bi4Ti3O12
Bi4Ti3O12+3BaCO3→3BaTiO3
first, Bi is weighed in a stoichiometric ratio2O3And TiO2Then adding Bi2O3And TiO2The mixture is uniformly mixed with KCl according to the mass ratio of 1: 1; then carrying out molten salt reaction to prepare Bi4Ti3O12；
Next, Bi was weighed in a stoichiometric ratio4Ti3O12And BaCO3Then adding Bi4Ti3O12And BaCO3With KCl according to 1: 1.5, uniformly mixing; then carrying out molten salt reaction, and finally washing by water,Acid washing to obtain<001>CBaTiO3And (5) template.
CN201910930606.8A 2019-09-29 2019-09-29 High Tr-tAnd TcLead base of<001>CTextured piezoelectric ceramic material and preparation method thereof Pending CN110981480A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910930606.8A CN110981480A (en) 2019-09-29 2019-09-29 High Tr-tAnd TcLead base of<001>CTextured piezoelectric ceramic material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910930606.8A CN110981480A (en) 2019-09-29 2019-09-29 High Tr-tAnd TcLead base of<001>CTextured piezoelectric ceramic material and preparation method thereof

Publications (1)

Publication Number Publication Date
CN110981480A true CN110981480A (en) 2020-04-10

Family

ID=70081848

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910930606.8A Pending CN110981480A (en) 2019-09-29 2019-09-29 High Tr-tAnd TcLead base of<001>CTextured piezoelectric ceramic material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN110981480A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114436654A (en) * 2022-02-07 2022-05-06 哈尔滨工业大学 Relaxor ferroelectric lead-based ceramic material with high phase transition temperature, excellent fatigue resistance and high electromechanical performance, and preparation method and application thereof
CN115010483A (en) * 2022-06-29 2022-09-06 西安交通大学 Piezoelectric ceramic material insensitive to strain and components and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1647923A (en) * 2004-01-26 2005-08-03 精工爱普生株式会社 Piezoelectric element, piezoelectric actuator, ink jet recording head, ink jet printer
JP2007142261A (en) * 2005-11-21 2007-06-07 Seiko Epson Corp Piezoelectric element, piezoelectric actuator and ink-jet recording head
CN104987072A (en) * 2015-07-17 2015-10-21 哈尔滨工业大学 Lead indium niobate-lead magnesium niobate-lead titanate relaxor ferroelectric textured ceramic with high electrical properties and preparation method and application of textured ceramic
CN108358634A (en) * 2018-01-19 2018-08-03 淮阴工学院 Textured piezoelectric ceramic material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1647923A (en) * 2004-01-26 2005-08-03 精工爱普生株式会社 Piezoelectric element, piezoelectric actuator, ink jet recording head, ink jet printer
JP2007142261A (en) * 2005-11-21 2007-06-07 Seiko Epson Corp Piezoelectric element, piezoelectric actuator and ink-jet recording head
CN104987072A (en) * 2015-07-17 2015-10-21 哈尔滨工业大学 Lead indium niobate-lead magnesium niobate-lead titanate relaxor ferroelectric textured ceramic with high electrical properties and preparation method and application of textured ceramic
CN108358634A (en) * 2018-01-19 2018-08-03 淮阴工学院 Textured piezoelectric ceramic material and preparation method thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
DABIN LIN ET AL.: "Thermal stability and electric-field-induced strain behaviors for PIN-PSN-PT piezoelectric ceramics", 《J AM CERAM SOC.》 *
QIAN LI ET AL.: "Soft phonon modes and diffuse scattering in Pb(In1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3 relaxor ferroelectrics", 《JOURNAL OF MATERIOMICS》 *
惠增哲 等: "弛豫铁电单晶生长技术进展与现状", 《西安工业大学学报》 *
艾辽东，龙西法: "优化的Ｂ位离子氧化物共烧法制备钙钛矿结构的ＰＹＮ－ＰＺＮ－ＰＴ三元铁电陶瓷", 《湖北大学学报（自然科学版）》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114436654A (en) * 2022-02-07 2022-05-06 哈尔滨工业大学 Relaxor ferroelectric lead-based ceramic material with high phase transition temperature, excellent fatigue resistance and high electromechanical performance, and preparation method and application thereof
CN114436654B (en) * 2022-02-07 2022-10-28 哈尔滨工业大学 Relaxor ferroelectric lead-based ceramic material with high phase transition temperature, excellent fatigue resistance and high electromechanical performance, and preparation method and application thereof
CN115010483A (en) * 2022-06-29 2022-09-06 西安交通大学 Piezoelectric ceramic material insensitive to strain and components and preparation method and application thereof

Similar Documents

Publication Publication Date Title
CN109180181B (en) Lead-free relaxation antiferroelectric ceramic energy storage material and preparation method thereof
CN104961455B (en) A kind of textured piezoelectric ceramic material and preparation method thereof
CN102503413B (en) Textured (1-x-y) BNT-xBKT-yKNN ceramic material and preparation method thereof
CN111533556B (en) Preparation method of grain-oriented strontium sodium niobate leadless ferroelectric ceramic
CN109626988B (en) Piezoelectric ceramic material with high piezoelectric response and high Curie temperature and preparation method thereof
KR102308852B1 (en) BiScO3-PbTiO3 PIEZOELECTRIC MATERIAL COMPRISING BaTiO3 SEED LAYERS, AND METHOD OF FABRICATING THE SAME
CN110330332B (en) Low-temperature sintering piezoelectric ceramic material without sintering aid and preparation method thereof
CN109704762B (en) Strontium niobate-based antiferroelectric ceramic and preparation method and application thereof
CN110981480A (en) High Tr-tAnd TcLead base of&lt;001&gt;CTextured piezoelectric ceramic material and preparation method thereof
CN112745117A (en) Textured piezoelectric ceramic laminated driver and preparation method thereof
CN115093216A (en) Barium titanate doped lead-free ceramic with high electrostriction and low hysteresis and preparation method thereof
CN107903055B (en) Gradient doped sodium bismuth titanate based multilayer lead-free piezoelectric ceramic
CN102775142B (en) Lead-free electrostrictive ceramic material and preparation method thereof
CN113773078A (en) High-power piezoelectric ceramic material and preparation method thereof
CN111533555B (en) Preparation method of layered compact strontium potassium niobate leadless piezoelectric ceramic
US5788876A (en) Complex substituted lanthanum-lead-zirconium-titanium perovskite, ceramic composition and actuator
CN114315346A (en) Preparation method of large-strain lead-free piezoelectric textured ceramic with double-template texture
CN111499377B (en) Piezoelectric ceramic and preparation method thereof
CN113213918A (en) Strontium bismuth titanate-bismuth scandium acid-lead titanate series high-temperature piezoelectric ceramic material with high piezoelectric performance and low loss and preparation method thereof
CN105036736A (en) Sodium-bismuth-titanate-base lead-free electrostrictive ceramic material and preparation method thereof
CN110272277B (en) Piezoelectric material and preparation method thereof, and multilayer actuator and preparation method thereof
CN112759390A (en) Has high kpPSN-PZT piezoelectric ceramic and preparation method thereof
CN106986629B (en) Preparation method of bismuth titanate-based bismuth laminated structure ferroelectric ceramic target material
CN114478006A (en) KNNS-BNZ + CuO piezoceramic material and preparation method and application thereof
CN104098328A (en) Low-electric-field large-strain-response lead-free piezoelectric texture ceramic material as well as preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20200410