CN111807837B - Ferroelectric ceramic material, piezoelectric sensor and preparation method - Google Patents
Ferroelectric ceramic material, piezoelectric sensor and preparation method Download PDFInfo
- Publication number
- CN111807837B CN111807837B CN202010570411.XA CN202010570411A CN111807837B CN 111807837 B CN111807837 B CN 111807837B CN 202010570411 A CN202010570411 A CN 202010570411A CN 111807837 B CN111807837 B CN 111807837B
- Authority
- CN
- China
- Prior art keywords
- mixture
- powder
- putting
- ferroelectric
- ceramic material
- 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
- 229910002112 ferroelectric ceramic material Inorganic materials 0.000 title claims description 42
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 44
- 239000000203 mixture Substances 0.000 claims abstract description 42
- 238000000498 ball milling Methods 0.000 claims abstract description 36
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000007873 sieving Methods 0.000 claims abstract description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 10
- 238000007599 discharging Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 5
- 239000010935 stainless steel Substances 0.000 claims abstract description 5
- 239000012856 weighed raw material Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 17
- 229910010252 TiO3 Inorganic materials 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- 229910002971 CaTiO3 Inorganic materials 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000007306 turnover Effects 0.000 claims description 4
- 230000004888 barrier function Effects 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000005036 potential barrier Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 230000006870 function Effects 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008447 perception Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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
-
- 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
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
-
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
-
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
-
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/638—Removal 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
- 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
- C04B35/64—Burning or sintering processes
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/5116—Ag or Au
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/88—Metals
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/16—Measuring force or stress, in general using properties of piezoelectric devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/08—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of piezoelectric devices, i.e. electric circuits therefor
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/09—Forming piezoelectric or electrostrictive materials
- H10N30/093—Forming inorganic materials
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/09—Forming piezoelectric or electrostrictive materials
- H10N30/093—Forming inorganic materials
- H10N30/097—Forming inorganic materials by sintering
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/853—Ceramic compositions
- H10N30/8536—Alkaline earth metal based oxides, e.g. barium 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
- 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
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
-
- 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
- C04B2235/3215—Barium 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
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
- C04B2235/3234—Titanates, not containing zirconia
- C04B2235/3236—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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- 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
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Composite Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The preparation method comprises the steps of mixing weighed raw materials, putting the mixture into a ball milling tank for ball milling to form a mixture, putting the mixture into an oven for drying, and putting the mixture into a mortar for grinding and sieving to form powder; pre-burning the powder in a crucible at 1350 ℃ in a muffle furnace, grinding the pre-burned powder in a mortar into fine powder, adding polyvinyl alcohol resin with a predetermined mass fraction, uniformly mixing, and sieving to obtain secondary powder with the particle size of 0.15-0.28 mm; pouring the secondary powder into a stainless steel mold, and maintaining the pressure for a third preset time under a preset pressure to form a blank; and (3) placing the blank into a muffle furnace, raising the temperature to a preset temperature, preserving the heat for a fourth preset time, discharging polyvinyl alcohol resin to form a sample, placing the sample into a crucible, burying and burning the sample by using powder of the same material as an embedding material, and sintering the sample at the temperature of 1425 and 1475 ℃ to form a ceramic chip.
Description
Technical Field
The invention relates to the technical field of electronic ceramic materials, in particular to a ferroelectric ceramic material, a piezoelectric sensor and a preparation method.
Background
The piezoelectric material is a functional material which can stretch under the external applied voltage and generate voltage under the external applied force, and is an important sensing dielectric medium for realizing the conversion of mechanical signals and electric signals. The piezoelectric material is widely applied in the fields of modern industry and national defense, is an important perception material in a sensing system, and has an information support function which is more important for an intelligent system which develops at a high speed.
Pb (Ti, Zr) O is mostly adopted in the traditional piezoelectric material3(PZT) the piezoelectric coefficient d33 of the lead-free piezoelectric ceramic is about 400pC/N, but lead element in the system has strong toxicity, so that the lead-free piezoelectric ceramic generates biotoxicity harm and environmental pollution in preparation and scrap links. Therefore, the development of green piezoelectric materials to replace PZT application is needed. In order to solve the problem, a great deal of research is carried out on piezoelectric materials without lead elements in recent years, but performances such as a non-lead ceramic piezoelectric coefficient and the like are far lower than those of PZT materials. The reason is that in the traditional method for modifying the piezoelectric property of the ferroelectric ceramic, the adjustment and control are only carried out by two microstructures, namely lattice deformation and micron-sized large domain inversion, wherein the amplitude of the lattice deformation is small, and the potential barrier for the micron-sized large domain inversion is high.
This information disclosed in the background section is only for enhancement of understanding of the background of the invention and therefore it may contain information that does not form the prior art that is already known in this country to a person of ordinary skill in the art.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a ferroelectric ceramic material, a piezoelectric sensor and a preparation method. The piezoelectric material is based on component regulation and control, has a hierarchical nano electric domain structure, is provided with a large electric domain with a micron scale, is nested with a small electric domain with a nano scale, has high piezoelectric coefficient, is lead-free and green, is different from the traditional crystal lattice deformation and the large electric domain with the micron scale, has large overturning amplitude and small overturning potential barrier under an external force application field, and thus has a piezoelectric coefficient exceeding PZT in a macroscopic view, and d33 is up to 590 pC/N.
The purpose of the invention is realized by the following technical scheme.
In one aspect of the present invention, a ferroelectric ceramic material is composed of: (1-x) (Ba (Zr)0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3Wherein x is 42-56%, the ferroelectric ceramic material has a multi-level ferroelectric domain structure, and the ferroelectric ceramic material is prepared by adjusting xThe size of the multilayer ferroelectric domain structure is adjusted, and the ferroelectric ceramic material has a first preset range of turnover amplitude and a second preset range of turnover potential barrier under an external applied force field.
In the ferroelectric ceramic material, the multilevel ferroelectric domain structure comprises a nested structure of a first ferroelectric domain with the micron scale and a second ferroelectric domain with the scale of tens of nanometers.
Said ferroelectric ceramic material wherein said first predetermined range is greater than said second predetermined range.
In the ferroelectric ceramic material, the piezoelectric coefficient of the ferroelectric ceramic material is 590 pC/N.
According to another aspect of the present invention, a piezoelectric sensor is made via the ferroelectric ceramic material.
According to still another aspect of the present invention, a method for preparing the ferroelectric ceramic material comprises,
based on the chemical formula (1-x) (Ba (Zr)0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3The raw material BaCO is weighed according to the proportion of the elements3、CaTiO3、ZrO2And TiO2Wherein x is 0.40, 0.45, 0.50, 0.55, 0.60;
mixing the weighed raw materials, putting the mixture into a ball milling tank for ball milling to form a mixture, putting the mixture into an oven for drying, and putting the mixture into a mortar for grinding and sieving to form powder;
putting the powder into a crucible and pre-sintering in a muffle furnace at 1350 ℃, preserving heat for first preset time, naturally cooling to room temperature, and discharging;
grinding the presintered powder into fine powder in a mortar, filling the fine powder into a ball milling tank for secondary ball milling to form a secondary mixture, putting the secondary mixture into an oven for drying, grinding the secondary mixture in the mortar, adding polyvinyl alcohol resin with a predetermined mass fraction, uniformly mixing, and sieving to obtain secondary powder with the particle size of 0.15-0.28 mm;
putting the secondary powder into an oven for drying for a second preset time, pouring the secondary powder into a stainless steel mold, and maintaining the pressure at a preset pressure for a third preset time to form a blank;
putting the blank into a muffle furnace, heating to a preset temperature, preserving heat for a fourth preset time, discharging polyvinyl alcohol resin to form a sample,
and putting the sample into a crucible, burying and burning the sample by using powder made of the same material as the buried material, sintering the sample at the temperature of 1425-1475 ℃ to form a ceramic wafer, preserving the temperature for fifth preset time, and naturally cooling the ceramic wafer to the room temperature.
In the method, the ceramic wafer is polished smoothly, silver paste is coated on the upper surface and the lower surface, the ceramic wafer is placed in a furnace to be heated to 800 ℃, the temperature is kept for 20 minutes, and the ceramic wafer is naturally cooled to room temperature.
In the method, a ball milling solvent and agate balls are added into a ball milling tank, the ball milling solvent comprises absolute ethyl alcohol, ball milling is carried out for 4 hours, the ball milling rotating speed is 45 r/min, the mixture is put into an oven and dried for 3 hours at the temperature of 80 ℃, then the mixture is put into a mortar and ground, and the mixture is sieved by a 60-mesh sieve.
In the method, the preset mass fraction is 8%, the first preset time is 4 hours, the second preset time is 5-10 minutes, the third preset time is 90 seconds, the fourth preset time is 2 hours, the fifth preset time is 4 hours, the preset pressure is 30MPa, the preset temperature is 600 ℃ and the temperature is raised at the temperature raising speed of 5 ℃/min.
In the method, the chemical formula is 0.50(Ba (Zr)0.2Ti0.8)O3-0.50(Ba0.7Ca0.3)TiO3The sample was sintered at 1450 ℃ to form a ceramic wafer, the blank being cylindrical.
The description is only an outline of the technical solution of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention is implemented by those skilled in the art according to the content of the description, and in order to make the description and other objects, features and advantages of the present invention more obvious, the following is exemplified by the specific embodiments of the present invention.
Drawings
Various other advantages and benefits of the present invention will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. It is obvious that the drawings described below are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. Also, like parts are designated by like reference numerals throughout the drawings.
In the drawings:
FIG. 1 is a schematic transmission electron microscopy bright field image of a ferroelectric ceramic material according to one embodiment of the present invention;
FIG. 2 is a graph showing the variation of piezoelectric coefficient with BCT composition of a ferroelectric ceramic material according to an embodiment of the present invention.
The invention is further explained below with reference to the figures and examples.
Detailed Description
Specific embodiments of the present invention will be described in more detail below with reference to fig. 1 to 2. While specific embodiments of the invention are shown in the drawings, it should be understood that the invention may be embodied in various forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
It should be noted that certain terms are used throughout the description and claims to refer to particular components. As one skilled in the art will appreciate, various names may be used to refer to a component. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. The description which follows is a preferred embodiment of the invention, but is made for the purpose of illustrating the general principles of the invention and not for the purpose of limiting the scope of the invention. The scope of the present invention is defined by the appended claims.
For the purpose of facilitating an understanding of the embodiments of the present invention, the following description will be made in terms of several specific embodiments with reference to the accompanying drawings, and the drawings are not intended to limit the embodiments of the present invention.
As shown in fig. 1 to 2, a ferroelectric ceramic material is composed of:
(1-x)(Ba(Zr0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3wherein x is 42% -56%, and the ferroelectric ceramic material has a multi-level ferroelectric domain structure.
Preferably, the ferroelectric ceramic material consists of: (1-x) (Ba (Zr)0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3Wherein x is 42% -48%, and the formed multi-level ferroelectric domain structure has a nested structure of a first ferroelectric domain with micron scale and a second ferroelectric domain with 1-10 nm scale, so that the piezoelectric coefficient is maximized.
In a preferred embodiment of the ferroelectric ceramic material, the multilevel ferroelectric domain structure includes a nested structure of a first ferroelectric domain with a micron scale and a second ferroelectric domain with a tens of nanometers, and the ferroelectric ceramic material adjusts the multilevel ferroelectric domain structure by adjusting the size of x.
In a preferred embodiment of the ferroelectric ceramic material, the ferroelectric ceramic material has a first predetermined range of the switching amplitude and a second predetermined range of the switching barrier under an applied force field.
In a preferred embodiment of the ferroelectric ceramic material, the piezoelectric coefficient of the ferroelectric ceramic material is 590 pC/N.
The invention obtains a novel hierarchical nano ferroelectric domain structure by regulating and controlling components in barium titanate-based ceramics, and prepares a green piezoelectric material with ultrahigh piezoelectric coefficient.
In the preferred embodiment of the ferroelectric ceramic material, the raw material components and the mole percentage content of the ferroelectric ceramic material are (1-x) (Ba (Zr)0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3(x 42% -56%), implementing multiple levels by adjusting the size of xAnd a ferroelectric domain structure, thereby realizing the maximization of the piezoelectric coefficient.
In the preferred embodiment of the ferroelectric ceramic material, the raw material components and the mol percentage content thereof of the ferroelectric ceramic material are 0.50(Ba (Zr)0.2Ti0.8)O3-0.50(Ba0.7Ca0.3)TiO3，Abbreviated as BZT-50 BCT.
In the preferred embodiment of the ferroelectric ceramic material, the piezoelectric material BZT-50BCT has a multi-level ferroelectric domain structure. FIG. 1 is a transmission electron microscopy bright field image of a BZT-50BCT piezoelectric material of an embodiment of the invention. The graph shows that the piezoelectric material has a nested structure of a large ferroelectric domain with the scale of micron and a small ferroelectric domain with the scale of tens of nanometers, which is called a hierarchical nano ferroelectric domain structure.
In a preferred embodiment of the ferroelectric ceramic material, the first predetermined range is greater in value than the second predetermined range.
A piezoelectric sensor is made via the ferroelectric ceramic material.
In one embodiment, the piezoelectric sensor is a dynamic cable vibration detection piezoelectric sensor for marine use.
A method for preparing the ferroelectric ceramic material comprises the following steps,
based on the chemical formula (1-x) (Ba (Zr)0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3The raw material BaCO is weighed according to the proportion of the elements3、CaTiO3、ZrO2And TiO2Wherein x is 0.40, 0.45, 0.50, 0.55, 0.60;
mixing the weighed raw materials, putting the mixture into a ball milling tank for ball milling to form a mixture, putting the mixture into an oven for drying, and putting the mixture into a mortar for grinding and sieving to form powder;
putting the powder into a crucible and pre-sintering in a muffle furnace at 1350 ℃, preserving heat for first preset time, naturally cooling to room temperature, and discharging;
grinding the presintered powder into fine powder in a mortar, filling the fine powder into a ball milling tank for secondary ball milling to form a secondary mixture, putting the secondary mixture into an oven for drying, grinding the secondary mixture in the mortar, adding polyvinyl alcohol resin with a predetermined mass fraction, uniformly mixing, and sieving to obtain secondary powder with the particle size of 0.15-0.28 mm;
putting the secondary powder into an oven for drying for a second preset time, pouring the secondary powder into a stainless steel mold, and maintaining the pressure at a preset pressure for a third preset time to form a blank;
putting the blank into a muffle furnace, heating to a preset temperature, preserving heat for a fourth preset time, discharging polyvinyl alcohol resin to form a sample,
and putting the sample into a crucible, burying and burning the sample by using powder made of the same material as the buried material, sintering the sample at the temperature of 1425-1475 ℃ to form a ceramic wafer, preserving the temperature for fifth preset time, and naturally cooling the ceramic wafer to the room temperature.
In the preferred embodiment of the method, the ceramic wafer is polished smoothly, silver paste is coated on the upper surface and the lower surface, the ceramic wafer is placed in a furnace to be heated to 800 ℃, the temperature is kept for 20 minutes, and the ceramic wafer is naturally cooled to the room temperature.
In a preferred embodiment of the method, a ball-milling solvent and agate balls are added into a ball-milling tank, the ball-milling solvent comprises absolute ethyl alcohol, the ball-milling is carried out for 4 hours, the ball-milling rotation speed is 45 r/min, the mixture is put into an oven and dried for 3 hours at the temperature of 80 ℃, then the mixture is put into a mortar and ground, and the mixture is sieved by a 60-mesh sieve.
In a preferred embodiment of the method, the predetermined mass fraction is 8%, the first predetermined time is 4 hours, the second predetermined time is 5 to 10 minutes, the third predetermined time is 90 seconds, the fourth predetermined time is 2 hours, the fifth predetermined time is 4 hours, the predetermined pressure is 30MPa, the predetermined temperature is 600 ℃ and the temperature is raised at a rate of 5 ℃/min.
In a preferred embodiment of the process, the formula is 0.50(Ba (Zr)0.2Ti0.8)O3-0.50(Ba0.7Ca0.3)TiO3The sample was sintered at 1450 ℃ to form a ceramic wafer, the blank being cylindrical.
In one embodiment, the preparation method comprises the steps of:
weighing material
(1) According to the formula (1-x) (Ba (Zr)0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3Weighing BaCO as raw material according to the proportion of each element3，CaTiO3，ZrO2And TiO2Wherein x is 0.40, 0.45, 0.50, 0.55 and 0.60 respectively;
(2) mixing the weighed raw materials, putting the mixture into a ball milling tank, adding ball milling solvents of absolute ethyl alcohol and agate balls, carrying out ball milling for 4 hours at the ball milling rotating speed of 45 r/min, putting the mixture into an oven, drying the mixture for 3 hours at the temperature of 80 ℃, putting the mixture into a mortar, grinding the mixture, and sieving the mixture by using a 60-mesh sieve;
pre-firing
(3) Putting the powder treated in the step 2 into a crucible, compacting and covering; presintering in a muffle furnace at 1350 ℃, preserving heat for 4 hours, naturally cooling to room temperature, and discharging;
secondary ball milling
(4) Grinding the powder preburning in the step 3 into fine powder in a mortar, filling the fine powder into a ball milling tank, adding a ball milling medium, namely absolute ethyl alcohol, performing secondary ball milling at the rotating speed of 45 revolutions per minute for 8 hours, and putting the mixture into an oven to be dried at the temperature of 80 ℃;
granulating
(5) Grinding the powder dried in the step 4 in a mortar, adding PVA with the mass fraction of 8%, uniformly mixing, and sieving to obtain powder with the particle size of 0.15 mm-0.28 mm;
shaping of
(6) Drying the powder granulated in the step 5 in an oven for 5 to 10 minutes, weighing a certain amount of powder, pouring the powder into a stainless steel mold with the diameter of 10mm, and maintaining the pressure at 30MPa for 90 seconds to form a cylindrical blank;
glue discharging
(7) And (4) putting the blank in the step 6 into a muffle furnace, heating to 600 ℃, preserving the heat for 2 hours, and discharging PVA.
Sintering
(8) Putting the sample obtained in the step 7 into a crucible, burying and burning the sample by using the same powder as the buried material, sintering the sample at the temperature of 1425-1475 ℃, preserving the heat for 4 hours, and naturally cooling the sample to room temperature along with the furnace;
burning electrode
(9) Polishing the ceramic wafer fired in the step 8 to be smooth, coating silver paste on the upper surface and the lower surface, putting the ceramic wafer into a furnace, heating to 800 ℃, preserving heat for 20 minutes, and naturally cooling to room temperature;
(10) and testing the electric domain structure and the piezoelectric coefficient of the sample.
In one embodiment, the temperature rise rate of the piezoelectric material in step 7 is 5 ℃/min; the temperature rise rate in step 8 is 5 ℃/min.
Although the embodiments of the present invention have been described above with reference to the accompanying drawings, the present invention is not limited to the specific embodiments and the application fields, and the specific embodiments are illustrative, instructive, and not restrictive. Those skilled in the art, having the benefit of this disclosure, may effect numerous modifications thereto without departing from the scope of the invention as defined by the appended claims.
Claims (8)
1. A ferroelectric ceramic material, characterized in that the ferroelectric ceramic material consists of:
(1-x)(Ba(Zr0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3the multilayer ferroelectric ceramic material comprises a multilayer ferroelectric domain structure, the size of the multilayer ferroelectric domain structure is adjusted by the ferroelectric ceramic material, the ferroelectric ceramic material has a turnover amplitude in a first preset range and a turnover barrier in a second preset range under an external applied force field, the multilayer ferroelectric domain structure comprises a nested structure of a first ferroelectric domain with the scale of micron scale and a second ferroelectric domain with the scale of tens of nanometers, and the first preset range is larger than the second preset range in value.
2. A ferroelectric ceramic material according to claim 1, characterized in that: the piezoelectric coefficient of the ferroelectric ceramic material is 590 pC/N.
3. A piezoelectric sensor, characterized by: made via the ferroelectric ceramic material of any one of claims 1-2.
4. A method of preparing a ferroelectric ceramic material according to any one of claims 1-2, characterized in that: the method comprises the following steps of,
based on the chemical formula (1-x) (Ba (Zr)0.2Ti0.8)O3-x(Ba0.7Ca0.3)TiO3The raw material BaCO is weighed according to the proportion of the elements3、CaTiO3、ZrO2And TiO2Wherein x is 0.40, 0.45, 0.50, 0.55, 0.60;
mixing the weighed raw materials, putting the mixture into a ball milling tank for ball milling to form a mixture, putting the mixture into an oven for drying, and putting the mixture into a mortar for grinding and sieving to form powder;
putting the powder into a crucible and pre-sintering in a muffle furnace at 1350 ℃, preserving heat for first preset time, naturally cooling to room temperature, and discharging;
grinding the presintered powder into fine powder in a mortar, filling the fine powder into a ball milling tank for secondary ball milling to form a secondary mixture, putting the secondary mixture into an oven for drying, grinding the secondary mixture in the mortar, adding polyvinyl alcohol resin with a predetermined mass fraction, uniformly mixing, and sieving to obtain secondary powder with the particle size of 0.15-0.28 mm;
putting the secondary powder into an oven for drying for a second preset time, pouring the secondary powder into a stainless steel mold, and maintaining the pressure at a preset pressure for a third preset time to form a blank;
putting the blank into a muffle furnace, heating to a preset temperature, preserving heat for a fourth preset time, discharging polyvinyl alcohol resin to form a sample,
and putting the sample into a crucible, burying and burning the sample by using powder made of the same material as the buried material, sintering the sample at the temperature of 1425-1475 ℃ to form a ceramic wafer, preserving the temperature for fifth preset time, and naturally cooling the ceramic wafer to the room temperature.
5. The method of claim 4, wherein: polishing the ceramic wafer smoothly, coating silver paste on the upper surface and the lower surface, putting the ceramic wafer into a furnace, heating to 800 ℃, preserving heat for 20 minutes, and naturally cooling to room temperature.
6. The method of claim 4, wherein: adding a ball-milling solvent and agate balls into a ball-milling tank, ball-milling for 4 hours at the ball-milling rotating speed of 45 r/min, drying the mixture in an oven at 80 ℃ for 3 hours, grinding the mixture in a mortar, and sieving the mixture by a 60-mesh sieve.
7. The method of claim 4, wherein: the predetermined mass fraction is 8%, the first predetermined time is 4 hours, the second predetermined time is 5 to 10 minutes, the third predetermined time is 90 seconds, the fourth predetermined time is 2 hours, the fifth predetermined time is 4 hours, the predetermined pressure is 30MPa, the predetermined temperature is 600 ℃ and the temperature is raised at a rate of 5 ℃/min.
8. The method of claim 4, wherein: chemical formula is 0.50(Ba (Zr)0.2Ti0.8)O3-0.50(Ba0.7Ca0.3)TiO3The sample was sintered at 1450 ℃ to form a ceramic wafer, the blank being cylindrical.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010570411.XA CN111807837B (en) | 2020-06-19 | 2020-06-19 | Ferroelectric ceramic material, piezoelectric sensor and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010570411.XA CN111807837B (en) | 2020-06-19 | 2020-06-19 | Ferroelectric ceramic material, piezoelectric sensor and preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111807837A CN111807837A (en) | 2020-10-23 |
| CN111807837B true CN111807837B (en) | 2021-10-01 |
Family
ID=72846330
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010570411.XA Active CN111807837B (en) | 2020-06-19 | 2020-06-19 | Ferroelectric ceramic material, piezoelectric sensor and preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111807837B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116082038B (en) * | 2022-04-26 | 2023-12-22 | 西安交通大学 | Preparation method of novel ferroelectric ceramic |
| CN116003122A (en) * | 2023-01-10 | 2023-04-25 | 西安交通大学 | Piezoelectric ceramic based on reversible domain wall movement and preparation method and application thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439557B (en) * | 2015-12-14 | 2018-12-28 | 贵州大学 | A kind of barium titanate piezoelectric ceramics |
| CN106986634A (en) * | 2017-04-28 | 2017-07-28 | 信阳师范学院 | A kind of calcium barium zirconate titanate base piezoceramics and preparation method thereof |
-
2020
- 2020-06-19 CN CN202010570411.XA patent/CN111807837B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN111807837A (en) | 2020-10-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Bian et al. | Enhanced breakdown strength and energy density of antiferroelectric Pb, La (Zr, Sn, Ti) O3 ceramic by forming core-shell structure | |
| CN111807837B (en) | Ferroelectric ceramic material, piezoelectric sensor and preparation method | |
| KR101754292B1 (en) | Method for preparing BiFeO3-BaTiO3 ceramics having improved piezoelectric and ferroelectric properties and lead-free piezoelectric ceramics prepared thereby | |
| Ryu et al. | Effect of heating rate on the sintering behavior and the piezoelectric properties of lead zirconate titanate ceramics | |
| Takagi et al. | Ferroelectric and photostrictive properties of fine‐grained PLZT ceramics derived from mechanical alloying | |
| CN113880576B (en) | Low sintering temperature and anisotropic strontium barium niobate sodium tungsten bronze type piezoelectric ferroelectric ceramic material and preparation method thereof | |
| CN113321507B (en) | Doped modified lead-based piezoelectric ceramic with excellent and stable piezoelectric performance | |
| CN106977196B (en) | Non-stoichiometric bismuth sodium titanate-based ceramic and preparation method and application thereof | |
| US20200299197A1 (en) | Method for preparing dielectric having low dielectric loss and dielectric prepared thereby | |
| KR101786056B1 (en) | Lead-free piezoelectric seramic for low temperature firing having core-shell structure and method of manufacturing the same | |
| CN116606143B (en) | Piezoelectric ceramic material and preparation method thereof | |
| KR102627416B1 (en) | Method of fabricating ternary piezoeletric ceramics with improved piezoeletric properties | |
| Paik et al. | Sol-gel fabrication of samarium and manganese modified lead titanate thin films and ceramics | |
| CN115286386B (en) | Non-stoichiometric Nb 5+ Potassium sodium bismuth niobate tantalum zirconium iron acid ceramic and preparation method thereof | |
| KR20080108781A (en) | Composition and the manufacturing method of lead-free piezoelectric ceramics | |
| US3400076A (en) | Piezoelectric ceramic compositions | |
| Hansch et al. | The effects of the PbO content upon the microstructure and the ferroelectric properties of undoped sol-gel derived PZT (53/47) fibers | |
| CN108975910A (en) | A kind of sodium niobate base ferroelectric ceramics and its preparation method and application with temperature-stable electric field induced strain | |
| CN110963797B (en) | High-temperature giant electrostrictive ceramic material and preparation method thereof | |
| Singh et al. | Dielectric, ferroelectric and piezoelectric properties of La-modified PCT ceramics | |
| CN116477938B (en) | Barium titanate-based leadless piezoelectric ceramic and preparation method thereof | |
| KR101110365B1 (en) | Method for manufacturing ferroelectric ceramics | |
| CN116003122A (en) | Piezoelectric ceramic based on reversible domain wall movement and preparation method and application thereof | |
| KR100236185B1 (en) | Particulate lead titanate ceramic and method thereof | |
| JPH05139828A (en) | Production of piezoelectric ceramic |
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 |