CN114436652B - Lead zirconate titanate-lead niobium tantalum magnesium acid piezoelectric ceramic material and preparation method thereof - Google Patents
Lead zirconate titanate-lead niobium tantalum magnesium acid piezoelectric ceramic material and preparation method thereof Download PDFInfo
- Publication number
- CN114436652B CN114436652B CN202210108817.5A CN202210108817A CN114436652B CN 114436652 B CN114436652 B CN 114436652B CN 202210108817 A CN202210108817 A CN 202210108817A CN 114436652 B CN114436652 B CN 114436652B
- Authority
- CN
- China
- Prior art keywords
- lead
- ball milling
- equal
- zirconate titanate
- less
- 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.)
- Active
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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
- C04B35/491—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT
-
- 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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
- C04B35/491—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT
- C04B35/493—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT containing also other lead 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
-
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3213—Strontium oxides or oxide-forming salts thereof
-
- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
-
- 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
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
- C04B2235/3267—MnO2
-
- 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
- C04B2235/3294—Antimony oxides, antimonates, antimonites or oxide forming salts thereof, indium antimonate
-
- 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
- C04B2235/3296—Lead oxides, plumbates or oxide forming salts thereof, e.g. silver plumbate
Abstract
The invention discloses a lead zirconate titanate-niobium tantalum magnesium acid lead piezoelectric ceramic material and a preparation method thereof, wherein the material uses lead zirconate titanate Pb (Zr) u Ti 1‑u )O 3 The solid solution is taken as a main component, and a second component Pb (Mg 1/3 (Nb z Ta 1‑z ) 2/3 )O 3 Simultaneously doping antimony trioxide Sb 2 O 3 And manganese dioxide MnO 2 The method comprises the steps of carrying out a first treatment on the surface of the In Pb (Zr) u Ti 1‑u )O 3 The A site of (2) is doped with strontium ions to replace part of lead ions; the stoichiometric amount of the catalyst is (1-y) Pb 1‑x Sr x (Zr u Ti 1‑u )O 3 ‑yPb(Mg 1/3 (Nb z Ta 1‑z ) 2/3 )O 3 +v wt％Sb 2 O 3 +w wt％MnO 2 Wherein x and y are molar ratio, x is more than 0 and less than or equal to 0.3, y is more than 0 and less than or equal to 0.4, z is more than 0 and less than or equal to 0.8, u is more than or equal to 0.2 and less than or equal to 0.8, v is more than 0 and less than or equal to 0.4, and w is more than 0 and less than or equal to 0.2. The material has extremely low dielectric loss and dielectric constant, keeps better piezoelectric performance, and can greatly reduce energy loss in the process of realizing electromechanical conversion. At the same time, the material has a higher curie temperature, which makes it possible to use it in a wider temperature range.
Description
Technical Field
The invention relates to the field of piezoelectric ceramic materials, in particular to a lead zirconate titanate-lead niobium tantalum magnesium acid piezoelectric ceramic material and a preparation method thereof.
Background
With the wide application of piezoelectric ceramics in modern industrial life, piezoelectric ceramics with corresponding specific functions must be developed according to the demands of users in different use environments. In general, piezoelectric ceramics can be classified into two main classes according to their electrical properties: soft piezoelectric ceramics and hard piezoelectric ceramics. Soft piezoelectric ceramics are mainly characterized by high piezoelectric constant, low mechanical quality factor and high dielectric loss; whereas rigid piezoelectric ceramics are mainly characterized by a high mechanical quality factor, ultra-low dielectric loss, but generally have a relatively low piezoelectric constant.
The modification to improve the comprehensive electrical property of the piezoelectric ceramic has better research significance by adding multiple components and doping metal oxide.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a lead zirconate titanate-lead niobium tantalum magnesium acid piezoelectric ceramic material and a preparation method thereof, wherein the material has extremely low dielectric loss and dielectric constant, maintains good piezoelectric performance, and can greatly reduce energy loss in the process of realizing electromechanical conversion. At the same time, the material has a higher curie temperature, which makes it possible to use it in a wider temperature range.
For this purpose, the invention adopts the following technical scheme:
lead zirconate titanate-lead tantalum magnesium niobate piezoelectric ceramic material prepared from lead zirconate titanate Pb (Zr) u Ti 1-u )O 3 The solid solution is taken as a main component, and a second component Pb (Mg 1/3 (Nb z Ta 1-z ) 2/3 )O 3 Simultaneously doping antimony trioxide Sb 2 O 3 And manganese dioxide MnO 2 The method comprises the steps of carrying out a first treatment on the surface of the In Pb (Zr) u Ti 1-u )O 3 The A site of (2) is doped with strontium ions to replace part of lead ions; the stoichiometric amount of the catalyst is (1-y) Pb 1-x Sr x (Zr u Ti 1-u )O 3 -yPb(Mg 1/3 (Nb z Ta 1-z ) 2/3 )O 3 +v wt％Sb 2 O 3 +w wt％MnO 2 Wherein x and y are molar ratio, x is more than 0 and less than or equal to 0.3, and y is more than 0 and less than or equal to 0.4、0＜z≤0.8、0.2≤u≤0.8、0＜v≤0.4、0＜w≤0.2。
Based on the same inventive concept, the embodiment also provides a preparation method of the lead zirconate titanate-lead niobium tantalum magnesium titanate piezoelectric ceramic material, which comprises the following steps: s1, ball milling, namely weighing various raw materials according to stoichiometric amounts, mixing and ball milling to obtain ball grinding materials; s2, performing secondary ball milling, namely drying the ball milling material, performing presintering to obtain presintered powder, and performing secondary ball milling to the presintered powder to obtain a secondary ball grinding material; s3, forming, namely fully grinding the secondary ball milling material after drying, adding an adhesive for grinding and granulating to obtain granulated powder, and performing glue discharging treatment after the granulated powder is pressed and formed to obtain a ceramic blank; s4, sintering, namely sintering the ceramic blank to obtain a sintered ceramic sheet; s5, polarization: and polishing and printing electrodes on two sides of the sintered ceramic sheet, placing the sintered ceramic sheet in silicone oil, applying voltage for polarization, and obtaining the lead zirconate titanate-lead niobium tantalum magnesium acid lead piezoelectric ceramic material.
Preferably, in the step S1, the raw material includes strontium carbonate SrCO 3 Zirconium dioxide ZrO 2 Titanium oxide TiO 2 Antimony trioxide Sb 2 O 3 Magnesium oxide MgO, lead oxide Pb 3 O 4 Niobium pentoxide Nb 2 O 5 Tantalum pentoxide Ta 2 O 5 And manganese dioxide MnO 2 。
Preferably, in the step S1, zirconia balls are used as a medium, absolute ethyl alcohol is used as a solvent for ball milling, and the ball milling time is 18-30 hours; in the step S2, zirconia balls are used as a medium, absolute ethyl alcohol is used as a solvent for ball milling, and the secondary ball milling time is 10-16 hours.
Preferably, the pre-sintering temperature is 800-950 ℃ and the time is 1-3 hours.
Preferably, in the step S3, the binder is polyvinyl alcohol PVA, the mass of the binder is 8% of the total mass of the raw materials, and the pressure of the press molding is 1 to 3MPa.
Preferably, in the step S3, the temperature of the glue discharging treatment is 750 ℃ and the time is 2 hours.
Preferably, in the step S4, the sintering temperature is 1150-1250 ℃ and the sintering time is 1-3 hours.
Preferably, in the step S5, the sintered ceramic sheet polished on both sides is re-burned with silver as an electrode, and the temperature of the burning silver is 550 to 750 ℃ for 10 to 30 minutes.
Preferably, in the step S5, the temperature of polarization is 120-160 ℃, the electric field strength is 3-5 kV/mm, and the time is 20-40 minutes.
The technical scheme has the advantages that:
1. the material provided by the invention has extremely low dielectric loss and dielectric constant, keeps better piezoelectric performance, and can greatly reduce energy loss in the process of realizing electromechanical conversion;
2. the material provided by the invention can be prepared by adopting a traditional solid-phase reaction method, has simple and stable preparation process and convenient operation, is suitable for popularization of large-scale industrial production, and has practical application value and wide application prospect;
3. the material provided by the invention has higher Curie temperature, so that the material has the possibility of being applied in a wider temperature range, and has practical application value in high-temperature electronic devices.
Drawings
FIG. 1 is an XRD diffraction pattern of the material prepared in example one in the range of 20-80 degrees 2. Theta;
fig. 2 is a dielectric thermogram of the material prepared in example one.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, and in order to provide a more thorough understanding of the present invention, reference is made to the following detailed description of the invention in connection with the accompanying drawings and examples, in which the invention may be practiced in other ways than those described. Therefore, the invention is not limited by the specific implementations disclosed below.
Example 1
This example provides a zirconium titanatePreparation method of lead-niobium tantalum magnesium acid lead piezoelectric ceramic material, and preparation method accords with chemical composition of 0.98Pb 0.97 Sr 0.03 (Zr 0.52 Ti 0.48 )O 3 -0.02Pb(Mg 1/3 (Nb 0.8 Ta 0.2 ) 2/3 )O 3 +0.1wt％Sb 2 O 3 +0.1wt％MnO 2 Is a modified piezoelectric ceramic material.
The method of the embodiment comprises the following steps:
s1, ball milling, namely weighing analytically pure raw material SrCO according to the metering ratio 3 、ZrO 2 、TiO 2 、Sb 2 O 3 、MgO、Pb 3 0 4 、Nb 2 O 5 、Ta 2 O 5 And MnO 2 Mixing in absolute ethyl alcohol, putting into a ball milling tank, and barreling with zirconia balls for 30 hours to obtain ball grinding materials.
S2, performing secondary ball milling, namely drying absolute ethyl alcohol in the ball grinding material, and preserving heat for 3 hours at 800 ℃ for pre-sintering the dried powder to obtain pre-sintered powder. And (3) performing secondary ball milling on the presintered powder for 16 hours to obtain the secondary ball grinding material.
S3, forming, namely adding polyvinyl alcohol PVA solution into the secondary ball-milling material after drying, fully grinding until glue is uniformly dispersed, and granulating the added PVA solution with the mass of 8% of the total mass of the raw materials to obtain granulated powder. Pressing the granulated powder into small discs under 3Mpa, and preserving the temperature of the small discs at 750 ℃ for 2h for glue discharging treatment to obtain ceramic blanks.
S4, sintering, namely, preserving the temperature of the ceramic blank for 3 hours at 1150 ℃ to sinter, so as to obtain the sintered ceramic sheet.
S5, polarization: and polishing two sides of the sintered ceramic sheet, covering with silver paste, and performing silver burning treatment at 750 ℃ for 30 minutes. And placing the sintered ceramic sheet printed with the upper electrode in 160 ℃ environment, applying an electric field of 5kV/mm, and carrying out heat preservation for 40 minutes to carry out polarization treatment to obtain the material.
Example two
This example provides a method for preparing a lead zirconate titanate-lead tantalum magnesium niobate piezoelectric ceramic material, which is prepared to meet the chemical composition of 0.98Pb 0.97 Sr 0.03 (Zr 0.53 Ti 0.47 )O 3 -0.02Pb(Mg 1/3 (Nb 0.8 Ta 0.2 ) 2/3 )O 3 +0.1wt％Sb 2 O 3 +0.1wt％MnO 2 Is a modified piezoelectric ceramic material.
The method of the embodiment comprises the following steps:
s1, ball milling, namely weighing analytically pure raw material SrCO according to the metering ratio 3 、ZrO 2 、TiO 2 、Sb 2 O 3 、MgO、Pb 3 0 4 、Nb 2 O 5 、Ta 2 O 5 And MnO 2 Mixing in absolute ethyl alcohol, putting into a ball milling tank, and barreling with zirconia balls for 18 hours to obtain ball grinding materials.
S2, performing secondary ball milling, namely drying absolute ethyl alcohol in the ball grinding material, and preserving the heat of the dried powder for 1h at 950 ℃ to perform presintering to obtain presintered powder. And (3) performing secondary ball milling on the presintered powder for 10 hours to obtain the secondary ball grinding material.
S3, forming, namely adding polyvinyl alcohol PVA solution into the secondary ball-milling material after drying, fully grinding until glue is uniformly dispersed, and granulating the added PVA solution with the mass of 8% of the total mass of the raw materials to obtain granulated powder. Pressing the granulated powder into small discs under 1Mpa, and preserving the temperature of the small discs at 750 ℃ for 2 hours to perform glue discharging treatment to obtain ceramic blanks.
S4, sintering, namely, preserving the temperature of the ceramic body at 1250 ℃ for 3 hours, and sintering to obtain the sintered ceramic sheet.
S5, polarization: and polishing two sides of the sintered ceramic sheet, covering with silver paste, and performing silver burning treatment at 550 ℃ for 10 minutes. And placing the sintered ceramic sheet printed with the upper electrode in an environment of 120 ℃, applying an electric field of 3kV/mm, and preserving heat for 20 minutes to carry out polarization treatment to obtain the material.
Example III
This example provides a method for preparing a lead zirconate titanate-lead tantalum magnesium niobate piezoelectric ceramic material, which is prepared to meet the chemical composition of 0.98Pb 0.97 Sr 0.03 (Zr 0.52 Ti 0.48 )O 3 -0.02Pb(Mg 1/3 (Nb 0.8 Ta 0.2 ) 2/3 )O 3 +0.3wt％Sb 2 O 3 +0.1wt％MnO 2 Is a modified piezoelectric ceramic material.
The method of the embodiment comprises the following steps:
s1, ball milling, namely weighing analytically pure raw material SrCO according to the metering ratio 3 、ZrO 2 、TiO 2 、Sb 2 O 3 、MgO、Pb 3 0 4 、Nb 2 O 5 、Ta 2 O 5 And MnO 2 Mixing in absolute ethyl alcohol, putting into a ball milling tank, and barreling with zirconia balls for 30 hours to obtain ball grinding materials.
S2, performing secondary ball milling, namely drying absolute ethyl alcohol in the ball grinding material, and preserving the heat of the dried powder for 1h at 950 ℃ to perform presintering to obtain presintered powder. And (3) performing secondary ball milling on the presintered powder for 10 hours to obtain the secondary ball grinding material.
S3, forming, namely adding polyvinyl alcohol PVA solution into the secondary ball-milling material after drying, fully grinding until glue is uniformly dispersed, and granulating the added PVA solution with the mass of 8% of the total mass of the raw materials to obtain granulated powder. Pressing the granulated powder into small discs under 3Mpa, and preserving the temperature of the small discs at 750 ℃ for 2h for glue discharging treatment to obtain ceramic blanks.
S4, sintering, namely, preserving the temperature of the ceramic body at 1250 ℃ for 1h, and sintering to obtain the sintered ceramic sheet.
S5, polarization: and polishing two sides of the sintered ceramic sheet, covering with silver paste, and performing silver burning treatment at 750 ℃ for 10 minutes. And placing the sintered ceramic sheet printed with the upper electrode in 160 ℃ environment, applying an electric field of 5kV/mm, and preserving heat for 20 minutes to carry out polarization treatment to obtain the material.
Piezoelectric performance detection
The materials prepared in examples one to three were allowed to stand for 24 hours, and then the piezoelectric properties were measured, respectively, and the measurement results are shown in Table 1.
Table 1 results of piezoelectricity test of materials
XRD characterization
The XRD diffraction pattern of the material prepared in example one, in the range of 20-80 degrees 2 theta, with reference to figure 1, shows that the sample is in a single perovskite phase with no second phase present.
Characterization of dielectric Properties
The dielectric thermogram of the material prepared in example one, with reference to fig. 2, shows that the sample has a higher curie temperature, up to 376 ℃.
The lead zirconate titanate-lead tantalum magnesium niobate piezoelectric ceramic material provided by the invention has extremely low dielectric loss and dielectric constant, keeps better piezoelectric performance, and can greatly reduce energy loss in the process of realizing electromechanical conversion, thereby reducing noise floor output of the material on an electronic device and improving signal to noise ratio of the electronic device.
Meanwhile, the material has higher Curie temperature, so that the material has the possibility of being applied in a wider temperature range, and has practical application value in high-temperature electronic devices.
The lead zirconate titanate-lead tantalum magnesium niobate piezoelectric ceramic material provided by the invention can be prepared by adopting a traditional solid phase reaction method, has simple and stable preparation process and convenient operation, is suitable for popularization of large-scale industrial production, and has practical application value and wide application prospect.
It is to be understood that the above embodiments are merely illustrative of the application of the principles of the present invention, but not in limitation thereof. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the invention, and are also considered to be within the scope of the invention.
Claims (10)
1. A piezoelectric ceramic material of lead zirconate titanate-lead niobium tantalum magnesium acid is characterized in that Pb (Zr) zirconate titanate is used u Ti 1-u )O 3 The solid solution is taken as a main component, and a second component Pb (Mg 1/3 (Nb z Ta 1-z ) 2/3 )O 3 Simultaneously doping antimony trioxide Sb 2 O 3 And dioxygenManganese MnO 2 ；
In Pb (Zr) u Ti 1-u )O 3 The A site of (2) is doped with strontium ions to replace part of lead ions;
the stoichiometric amount of the catalyst is (1-y) Pb 1-x Sr x (Zr u Ti 1-u )O 3 -yPb(Mg 1/3 (Nb z Ta 1-z ) 2/3 )O 3
+v wt％Sb 2 O 3 +w wt％MnO 2 Wherein x and y are molar ratios, x=0.03, y=0.02, z=0.8, u=0.52, v=0.1, w=0.1;
the piezoelectric ceramic material is prepared by adopting a solid phase reaction method, and the sintering temperature is 1150-1250 ℃.
2. A method for preparing the lead zirconate titanate-lead tantalum magnesium niobate piezoelectric ceramic material according to claim 1, comprising the steps of:
s1, ball milling, namely weighing various raw materials according to stoichiometric amounts, mixing and ball milling to obtain ball grinding materials;
s2, performing secondary ball milling, namely drying the ball milling material, performing presintering to obtain presintered powder, and performing secondary ball milling to the presintered powder to obtain a secondary ball grinding material;
s3, forming, namely fully grinding the secondary ball milling material after drying, adding an adhesive for grinding and granulating to obtain granulated powder, and performing glue discharging treatment after the granulated powder is pressed and formed to obtain a ceramic blank;
s4, sintering, namely sintering the ceramic blank to obtain a sintered ceramic sheet;
s5, polarization: and polishing and printing electrodes on two sides of the sintered ceramic sheet, placing the sintered ceramic sheet in silicone oil, applying voltage for polarization, and obtaining the lead zirconate titanate-lead niobium tantalum magnesium acid lead piezoelectric ceramic material.
3. The method according to claim 2, wherein in the step S1, the raw material comprises strontium carbonate SrCO 3 Zirconium dioxide ZrO 2 Titanium oxide TiO 2 Antimony trioxide Sb 2 O 3 Magnesium oxide MgO, lead oxide Pb 3 O 4 Niobium pentoxide Nb 2 O 5 Tantalum pentoxide Ta 2 O 5 And manganese dioxide MnO 2 。
4. The preparation method according to claim 2, wherein in the step S1, zirconia balls are used as a medium, absolute ethyl alcohol is used as a solvent for ball milling, and the ball milling time is 18-30 hours;
in the step S2, zirconia balls are used as a medium, absolute ethyl alcohol is used as a solvent for ball milling, and the secondary ball milling time is 10-16 hours.
5. The method according to claim 2, wherein the pre-sintering is performed at a temperature of 800 to 950 ℃ for a time of 1 to 3 hours.
6. The method according to claim 2, wherein in the step S3, the binder is polyvinyl alcohol PVA, the mass of the binder is 8% of the total mass of the raw materials, and the pressure of the press molding is 1 to 3MPa.
7. The method according to claim 2, wherein in the step S3, the temperature of the adhesive removing treatment is 750 ℃ for 2 hours.
8. The method according to claim 2, wherein in the step S4, the sintering time is 1 to 3 hours.
9. The method according to claim 2, wherein in the step S5, silver is burned again by silver as an electrode on the sintered ceramic sheet polished on both sides, and the temperature of the burning silver is 550 to 750 ℃ for 10 to 30 minutes.
10. The method according to claim 2, wherein in the step S5, the temperature of polarization is 120 to 160 ℃, the electric field strength is 3 to 5kV/mm, and the time is 20 to 40 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210108817.5A CN114436652B (en) | 2022-01-28 | 2022-01-28 | Lead zirconate titanate-lead niobium tantalum magnesium acid piezoelectric ceramic material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210108817.5A CN114436652B (en) | 2022-01-28 | 2022-01-28 | Lead zirconate titanate-lead niobium tantalum magnesium acid piezoelectric ceramic material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114436652A CN114436652A (en) | 2022-05-06 |
| CN114436652B true CN114436652B (en) | 2023-05-16 |
Family
ID=81371759
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210108817.5A Active CN114436652B (en) | 2022-01-28 | 2022-01-28 | Lead zirconate titanate-lead niobium tantalum magnesium acid piezoelectric ceramic material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114436652B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107117965A (en) * | 2017-05-18 | 2017-09-01 | 四川大学 | Doped modified lead nickelate-lead zirconate titanate piezoelectric ceramic and preparation method thereof |
Family Cites Families (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54137009A (en) * | 1978-04-17 | 1979-10-24 | Tdk Electronics Co Ltd | High dielectric ceramic composition |
| JPS61256959A (en) * | 1985-05-02 | 1986-11-14 | ティーディーケイ株式会社 | High permittivity ceramic composition |
| JPH0788253B2 (en) * | 1986-06-18 | 1995-09-27 | 日立金属株式会社 | Piezoelectric composition |
| CN1006941B (en) * | 1988-02-06 | 1990-02-21 | 清华大学 | Low-temp. sintered leady piezoelectric ceramic and its manufacture technology |
| JPH0772088B2 (en) * | 1991-04-19 | 1995-08-02 | 株式会社コロイドリサーチ | Method for producing complex oxide precursor powder |
| JP4370135B2 (en) * | 2003-09-10 | 2009-11-25 | 日本セラミック株式会社 | Piezoelectric ceramic composition |
| CN101215168B (en) * | 2008-01-16 | 2010-06-02 | 武汉理工大学 | Doping modifying method for lead magnesio-tantalate lead zirconate lead titanate |
| CN103145415A (en) * | 2012-09-24 | 2013-06-12 | 天津大学 | Low-temperature sintered high-power antimony manganese-lead zirconate titanate piezoelectric ceramics |
| CN102924082A (en) * | 2012-10-22 | 2013-02-13 | 南京航空航天大学 | Manganese-doped niobium nickel-lead zirconate titanate piezoelectric ceramic and preparation method thereof |
| CN103304235B (en) * | 2013-03-01 | 2015-11-25 | 苏州市职业大学 | A kind of production method of thin brilliant high strength PMN-PZT piezoceramic material |
| CN103964846B (en) * | 2014-04-29 | 2015-12-09 | 常州市斯威芙特制针科技有限公司 | Piezoelectric bimorph piezoceramic material and preparation method thereof |
| CN106220169B (en) * | 2016-07-14 | 2019-08-16 | 重庆胜普昂凯科技有限公司 | Modified lead nickle niobate-lead titanate piezoelectric ceramics and preparation method thereof |
| CN107986782B (en) * | 2017-11-21 | 2020-01-03 | 歌尔股份有限公司 | Doped modified lead zirconate titanate piezoelectric ceramic and preparation method thereof |
| CN109437895B (en) * | 2018-11-26 | 2021-08-31 | 中国电子科技集团公司第四十六研究所 | Preparation method of lead zirconate titanate-lead magnesium niobate piezoelectric ceramic |
| CN112174663B (en) * | 2020-09-21 | 2022-10-18 | 李茂洪 | High-performance piezoelectric ceramic and preparation method thereof |
-
2022
- 2022-01-28 CN CN202210108817.5A patent/CN114436652B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107117965A (en) * | 2017-05-18 | 2017-09-01 | 四川大学 | Doped modified lead nickelate-lead zirconate titanate piezoelectric ceramic and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Characteristics and structure of Mn-doped (0.6 − x)PMT–0.4PT–xPZ(x=0.2,0.25) ternary system near morphotropic phase boundary;Qiu ZX等;《JOURNAL OF MATERIALS SCIENCE-MATERIALS IN ELECTRONICS》;第14261-14266页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114436652A (en) | 2022-05-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107986782B (en) | Doped modified lead zirconate titanate piezoelectric ceramic and preparation method thereof | |
| JP4513948B2 (en) | Piezoelectric ceramic and manufacturing method thereof | |
| CN113213930B (en) | Multi-element doped potassium-sodium niobate-based piezoelectric ceramic and preparation method thereof | |
| CN103342556A (en) | Preparation method of two-phase low-temperature co-sintered temperature stable dielectric ceramic material | |
| CN111233470B (en) | Antiferroelectric ceramic material with excellent charge and discharge performance and preparation method thereof | |
| CN111087238B (en) | Sodium bismuth titanate based leadless piezoelectric ceramic and preparation method thereof | |
| CN101805185A (en) | Method for preparing leadmagnesio-niobate lead titanate relaxation ferroelectric ceramics | |
| CN111269009A (en) | Bismuth zirconate manganate-bismuth scandate-lead titanate series piezoelectric ceramic material and preparation method thereof | |
| CN116573936B (en) | Anion modified piezoelectric ceramic and preparation method thereof | |
| US20140339458A1 (en) | Piezoelectric ceramic and piezoelectric device containing the same | |
| CN102167585A (en) | Multielement-doped bismuth titanate group lead-free piezoceramic material and preparation method thereof | |
| CN114455944B (en) | Bismuth layer-structured piezoelectric ceramic material and preparation method thereof | |
| CN101774803A (en) | A (Ba, sr) TiO3-based ceramic medium and its prepn | |
| KR101333792B1 (en) | Bismuth-based pb-free piezoelectric ceramics and method of fabricating the same | |
| CN113582667B (en) | Low-temperature cofiring high-energy-storage antiferroelectric ceramic material and preparation method and application thereof | |
| US20120112607A1 (en) | Ceramic composition for piezoelectric actuator and piezoelectric actuator including the same | |
| CN112876240B (en) | Ceramic material and preparation method and application thereof | |
| CN114436652B (en) | Lead zirconate titanate-lead niobium tantalum magnesium acid piezoelectric ceramic material and preparation method thereof | |
| CN114685187B (en) | Method for improving equivalent flexoelectric response of composite ceramic | |
| CN114478006A (en) | KNNS-BNZ + CuO piezoceramic material and preparation method and application thereof | |
| CN113800904A (en) | High-energy low-loss BNT-SBT-xSMN ceramic material and preparation method thereof | |
| CN113149644A (en) | Low-temperature sintered lead antimonate manganese-lead zirconate titanate low-dielectric-loss piezoelectric ceramic and preparation method thereof | |
| CN116120054B (en) | Bismuth calcium titanate-based piezoelectric ceramic material and preparation method thereof | |
| CN114447208A (en) | Piezoelectric ceramic material, preparation method and application | |
| CN114436653B (en) | Anti-reduction potassium-sodium niobate based lead-free piezoelectric ceramic with fatigue resistance, high inverse voltage resistance and high stability and preparation method 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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |