CN107151138B - Low-loss ultrahigh-voltage-performance lead-free piezoelectric ceramic material and preparation method thereof - Google Patents
Low-loss ultrahigh-voltage-performance lead-free piezoelectric ceramic material and preparation method thereof Download PDFInfo
- Publication number
- CN107151138B CN107151138B CN201710301046.0A CN201710301046A CN107151138B CN 107151138 B CN107151138 B CN 107151138B CN 201710301046 A CN201710301046 A CN 201710301046A CN 107151138 B CN107151138 B CN 107151138B
- Authority
- CN
- China
- Prior art keywords
- ceramic material
- hours
- ultrahigh
- loss
- crystal phase
- 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.)
- Expired - Fee Related
Links
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims description 16
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 238000003801 milling Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 229910052573 porcelain Inorganic materials 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Inorganic materials [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- 230000005684 electric field Effects 0.000 claims description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 238000000576 coating method Methods 0.000 abstract description 7
- 239000011248 coating agent Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000008859 change Effects 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000010287 polarization Effects 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000000919 ceramic Substances 0.000 description 10
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- 238000002059 diagnostic imaging Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten(VI) oxide Inorganic materials O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
- C04B35/46—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 titanium oxides or titanates
- C04B35/462—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 titanium oxides or titanates based on titanates
- C04B35/465—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on 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
- 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
- C04B35/63—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
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
-
- 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
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- 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
- C04B41/515—Other specific metals
-
- 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
-
- 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
-
- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3258—Tungsten oxides, tungstates, 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
- C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
-
- 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
- C04B2235/70—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)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a low-loss ultrahigh-voltage performance lead-free piezoelectric ceramic material and a preparation method thereof, and the formula comprises the following components: 0.95Ba (Ti)0.89Sn0.11)O3‑0.05Bi2WO6+0.5% Mn +0.5% Cu by addition of Bi2WO6Promoting sintering to obtain compact and homogeneous crystal grain ceramic material, and combining chemical coating process to synthesize 0.95Ba (Ti)0.89Sn0.11)O3The Mn/Cu surface coating particles are obtained by a chemical coating method on the particle surface, a gradient hierarchical structure is formed during synthesis, the valence change of Sn is inhibited, the problem of high leakage current of the system is solved, the piezoelectric performance is improved, the dielectric loss is reduced, and the problems of poor insulativity, difficulty in polarization and the like of the system are solved. The ceramic material has ultrahigh voltage performance, ultralow dielectric loss, environmental friendliness and good stability.
Description
Technical Field
The invention relates to a lead-free piezoelectric ceramic material, in particular to an ABO3Lead-free piezoelectric ceramic with a perovskite structure and low loss and ultrahigh piezoelectric performance and a preparation method thereof.
Background
Piezoelectric ceramics are information functional ceramic materials capable of mutually converting mechanical energy and electric energy, have piezoelectricity, dielectricity, elasticity and the like, and are widely applied to medical imaging, acoustic sensors, acoustic transducers, ultrasonic motors and the like. The piezoelectric ceramic material used at present is mainly lead-based piezoelectric ceramic, but the content of PbO in the lead-based piezoelectric ceramic accounts for about 70% of the total amount of raw materials, the lead-based piezoelectric material can bring serious harm to human and ecological environment in the processes of production, use and waste post-treatment, lead dissolved in acid rain can directly or indirectly invade human bodies through water, animals and plants, and the lead mainly influences the nervous systems of the human bodies. With the increasing awareness of environmental protection, lead-free research for replacing electronic ceramic materials represented by conventional lead-based ceramic materials has become one of the hot spots in the material field in recent years. However, the comprehensive performance of the currently researched lead-free piezoelectric ceramic system can not reach the level of lead-based ceramic, and the lead-based piezoelectric ceramic system can not be substituted for the lead-based ceramic to meet the requirements of practical application. In particular, in the modification of lead-free piezoelectric ceramics, the improvement of piezoelectric performance is always accompanied by an increase in dielectric loss.
Disclosure of Invention
The invention aims to provide an ABO3The perovskite structure has ultrahigh voltage performance, ultralow dielectric loss, environment friendliness and good stability, and the preparation method thereof.
The invention relates to a low-loss lead-free piezoelectric ceramic material with ultrahigh piezoelectric property, which comprises the following components in percentage by weight:
0.95Ba(Ti0.89Sn0.11)O3-0.05Bi2WO6+0.5%Mn+0.5%Cu ；
by adding Bi2WO6Promoting sintering to obtain compact and homogeneous crystal grain ceramic material, and combining chemical coating process to synthesize 0.95Ba (Ti)0.89Sn0.11)O3The Mn/Cu surface coating particles are obtained by a chemical coating method on the particle surface, a gradient hierarchical structure is formed during synthesis, the valence change of Sn is inhibited, the problem of high leakage current of the system is solved, the piezoelectric performance is improved, the dielectric loss is reduced, and the problems of poor insulativity, difficulty in polarization and the like of the system are solved.
The preparation method of the low-loss ultrahigh-voltage lead-free piezoelectric ceramic material comprises the following steps:
(1) to analytically pure BaCO3、Bi2O3、CaCO3、SnO2、WO3、TiO2As raw material, according to the chemical formula 0.95Ba (Ti)0.89Sn0.11)O3-0.05Bi2WO6Burdening and uniformly mixing;
(2) putting the uniformly mixed raw materials into a ball milling tank, carrying out ball milling for 24 hours by taking zirconium oxide as a milling ball and absolute ethyl alcohol as a medium, separating the milling ball, and drying; pressing the dried powder into a large block blank, and keeping the temperature of 1050 ℃ in a high-aluminum crucible for 2 hours to synthesize a main crystal phase;
(3) pulverizing the synthesized main crystal phase, and mixing with Mn (NO)3)2、Cu(NO3)2Solution according to 0.95Ba (Ti)0.89Sn0.11)O3-0.05Bi2WO6+0.5% of Mn +0.5% of Cu, stirring and mixing uniformly, dripping ammonia water to form a precipitate on the surface of the particles, and performing suction filtration and cleaning;
(4) drying the raw materials after suction filtration and cleaning, and then preserving heat for 2 hours in a high-aluminum crucible at 950 ℃ to synthesize a main crystal phase with a graded gradient structure;
(5) crushing the main crystal phase synthesized in the step (4), performing secondary ball milling for 24 hours, drying, and adding a PVA solution with the mass of 5% of the raw material for granulation;
(6) after granulation, pressing and forming in a steel die under 150 MPa;
(7) the formed raw materials are sintered into porcelain after being insulated for 2 hours at 1250 ℃, and electrodes are plated on two surfaces of the porcelain;
(8) polarizing in silicone oil, polarizing in electric field 3000V/mm at 30 deg.C for 30 min, and cooling to room temperature.
The obtained product has excellent piezoelectric performance through experimental measurementd 33The material has the advantages of =820 pC/N, high dielectric constant, low dielectric loss (tan = 0.78%), good stability and low cost, is suitable for industrial production, and can be used in the field of ultrasonic transducers.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited thereto.
Examples
The preparation method of the low-loss ultrahigh-voltage lead-free piezoelectric ceramic material comprises the following steps:
(1) analytically pure BaCO3, Bi2O3, CaCO3, SnO2, WO3 and TiO2 are used as raw materials, and the raw materials are mixed and evenly mixed according to a chemical formula of 0.95Ba (Ti0.89Sn0.11) O3-0.05Bi2WO 6;
(2) putting the uniformly mixed raw materials into a ball milling tank, ball milling for 24 hours by taking zirconium oxide as a milling ball and absolute ethyl alcohol as a medium, separating the milling ball, and drying at 80 ℃; pressing the dried powder into a large block blank, and keeping the temperature of 1050 ℃ in a high-aluminum crucible for 2 hours to synthesize a main crystal phase;
(3) pulverizing the synthesized main crystal phase, and mixing with Mn (NO)3)2、Cu(NO3)2Solution according to 0.95Ba (Ti)0.89Sn0.11)O3-0.05Bi2WO6+0.5% of Mn +0.5% of Cu, stirring and mixing uniformly, dripping ammonia water to form a precipitate on the surface of the particles, and performing suction filtration and cleaning;
(4) drying the raw materials after suction filtration and cleaning at 120 ℃, and then preserving heat for 2 hours at 950 ℃ in a high-alumina crucible to synthesize a main crystalline phase with a graded gradient structure;
(5) crushing the main crystal phase synthesized in the step (4), performing secondary ball milling for 24 hours, drying, and adding a PVA solution with the mass of 5% of the raw material for granulation;
(6) after granulation, pressing and forming in a steel die under 150 MPa;
(7) keeping the temperature of the formed plain sheet at 600 ℃ for 2h at the heating rate of 100 ℃/h for removing glue, keeping the temperature at 1250 ℃ for 2h, processing the sintered sample into a sheet with two smooth surfaces and the thickness of about 1mm, and coating a silver electrode;
(8) polarizing in silicone oil, polarizing in electric field 3000V/mm at 30 deg.C for 30 min, and cooling to room temperature.
The piezoelectric property of the piezoelectric ceramic was measured by IRE standard after the obtained product was left to stand for 24 hours.
The performance measurements are as follows:
Claims (1)
1. a low-loss ultrahigh-voltage-performance lead-free piezoelectric ceramic material is characterized in that: the preparation method of the ceramic material comprises the following steps:
(1) to analytically pure BaCO3、Bi2O3、SnO2、WO3、TiO2As raw material, according to the chemical formula 0.95Ba (Ti)0.89Sn0.11)O3-0.05Bi2WO6Burdening and uniformly mixing;
(2) putting the uniformly mixed raw materials into a ball milling tank, carrying out ball milling for 24 hours by taking zirconium oxide as a milling ball and absolute ethyl alcohol as a medium, separating the milling ball, and drying; pressing the dried powder into a large block blank, and keeping the temperature of 1050 ℃ in a high-aluminum crucible for 2 hours to synthesize a main crystal phase;
(3) pulverizing the synthesized main crystal phase, and mixing with Mn (NO)3)2、Cu(NO3)2Solution according to 0.95Ba (Ti)0.89Sn0.11)O3-0.05Bi2WO6+0.5% of Mn +0.5% of Cu, stirring and mixing uniformly, dripping ammonia water to form a precipitate on the surface of the particles, and performing suction filtration and cleaning;
(4) drying the raw materials after suction filtration and cleaning, and then preserving heat for 2 hours in a high-aluminum crucible at 950 ℃ to synthesize a main crystal phase with a graded gradient structure;
(5) crushing the main crystal phase synthesized in the step (4), performing secondary ball milling for 24 hours, drying, and adding a PVA solution with the mass of 5% of the raw material for granulation;
(6) after granulation, pressing and forming in a steel die under 150 MPa;
(7) the formed raw materials are sintered into porcelain after being insulated for 2 hours at 1250 ℃, and electrodes are plated on two surfaces of the porcelain;
(8) polarizing in silicone oil, polarizing at 3000V/mm electric field and 30 deg.C for 30 min, and cooling to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710301046.0A CN107151138B (en) | 2017-05-02 | 2017-05-02 | Low-loss ultrahigh-voltage-performance lead-free piezoelectric ceramic material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710301046.0A CN107151138B (en) | 2017-05-02 | 2017-05-02 | Low-loss ultrahigh-voltage-performance lead-free piezoelectric ceramic material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107151138A CN107151138A (en) | 2017-09-12 |
| CN107151138B true CN107151138B (en) | 2020-07-10 |
Family
ID=59794032
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710301046.0A Expired - Fee Related CN107151138B (en) | 2017-05-02 | 2017-05-02 | Low-loss ultrahigh-voltage-performance lead-free piezoelectric ceramic material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107151138B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108689703B (en) * | 2018-06-26 | 2021-01-05 | 桂林电子科技大学 | Lead-free ferroelectric ceramic material with giant dielectric constant and electric tuning characteristics and preparation method thereof |
| CN109265167B (en) * | 2018-09-05 | 2021-04-20 | 佛山市亿强电子有限公司 | Method for sintering PZT piezoelectric ceramic at low temperature and piezoelectric ceramic |
| CN111747738B (en) * | 2020-06-19 | 2021-07-06 | 西安交通大学 | Preparation method of gradient ceramic piezoelectric material, piezoelectric material and piezoelectric sensor |
| CN114478007A (en) * | 2022-02-17 | 2022-05-13 | 同济大学 | Sodium niobate-based ceramic material with good process tolerance, high piezoelectric property and high dielectric property, and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1604246A (en) * | 2004-11-08 | 2005-04-06 | 华南理工大学 | Fine crystal ceramic capacitor dielectric material with high dielectric coefficient and process for preparing same |
| CN102030529A (en) * | 2010-11-17 | 2011-04-27 | 合肥工业大学 | Bismuth-containing complex perovskite-lead zirconate titanate quasi-ternary system piezoelectric ceramic and preparation method thereof |
| CN105884350A (en) * | 2016-04-08 | 2016-08-24 | 江苏大学 | Barium calcium zirconate titanate leadless piezoelectric ceramic material and preparation method thereof |
-
2017
- 2017-05-02 CN CN201710301046.0A patent/CN107151138B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1604246A (en) * | 2004-11-08 | 2005-04-06 | 华南理工大学 | Fine crystal ceramic capacitor dielectric material with high dielectric coefficient and process for preparing same |
| CN102030529A (en) * | 2010-11-17 | 2011-04-27 | 合肥工业大学 | Bismuth-containing complex perovskite-lead zirconate titanate quasi-ternary system piezoelectric ceramic and preparation method thereof |
| CN105884350A (en) * | 2016-04-08 | 2016-08-24 | 江苏大学 | Barium calcium zirconate titanate leadless piezoelectric ceramic material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Polarization switching and high piezoelectric response in Sn-modified BaTiO3;Ajay Kumar Kalyani等;《American Physical Society》;20150105;第91卷;第024101-1页-第024101-13页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107151138A (en) | 2017-09-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107151138B (en) | Low-loss ultrahigh-voltage-performance lead-free piezoelectric ceramic material and preparation method thereof | |
| CN103030390B (en) | Zinc oxide piezoresistor material and preparation method | |
| CN102531578A (en) | BCT-BZT-BST (Barium calcium titanate-barium zirconate titanate-barium stannate titanate) ternary system lead-free piezoelectric ceramic | |
| CN103214238B (en) | Preparation method of barium strontium titanate dielectric temperature stable ceramic capacitor material | |
| CN110128127B (en) | Bismuth ferrite-barium titanate-based lead-free piezoelectric ceramic with high piezoelectric performance and high-temperature stability and preparation method thereof | |
| CN102167585B (en) | Multielement-doped bismuth titanate group lead-free piezoceramic material and preparation method thereof | |
| CN113200744A (en) | Lead-free piezoelectric ceramic sensor material and preparation method thereof | |
| CN102285792B (en) | Lead-free piezoelectric ceramic with perovskite structure | |
| CN104030679A (en) | BaTiO3-based lead-free PTC (positive temperature coefficient) thermistor ceramic material sintered in reducing atmosphere and preparation method thereof | |
| CN103833354A (en) | Solid solution-modified sodium bismuth titanate leadless piezoelectric ceramics and preparation method thereof | |
| CN102320828B (en) | Unleaded piezoelectric ceramic consisting of B-site composite Bi-based compound and preparation method thereof | |
| CN101983949B (en) | White opaque glaze for piezoelectric ceramic atomizing sheet and preparation method thereof | |
| CN110128128B (en) | Bismuth ferrite-bismuth aluminate-bismuth zinc titanate high-temperature piezoelectric ceramic with zero temperature coefficient and high-temperature stability and preparation method thereof | |
| CN102199036A (en) | Method for preparing energy storage ceramic with high breakdown strength | |
| CN100360466C (en) | Doped and modified piezoelectric ceramic of potassium sodium bismuth titanate and preparation method | |
| CN103288450B (en) | Potassium-sodium niobate-bismuth potassium zirconate-titanate/lithium-base leadless piezoelectric ceramic | |
| CN107032784A (en) | A kind of big Piezoelectric Anisotropy lead-free piezoceramic material and preparation method thereof | |
| CN107903055B (en) | Gradient doped sodium bismuth titanate based multilayer lead-free piezoelectric ceramic | |
| CN103693957A (en) | Method for preparing microwave dielectric ceramic material | |
| CN107098701B (en) | Potassium sodium lithium niobate-potassium sodium bismuth zirconate-bismuth acid bismuth ternary system lead-free piezoelectric ceramic | |
| CN102351533A (en) | Calcium barium zirconate titanate based leadless piezoelectric ceramics with low temperature sintering and high piezoelectric properties and preparation method thereof | |
| CN101798214A (en) | (Na1/2Bi1/2) TiO3/BaTiO3 ceramic dielectric material and preparation of capacitor thereof | |
| CN106518058A (en) | Lead-free compound ferroelectric ceramic composed of potassium-bismuth titanate and zinc oxide and preparation thereof | |
| KR101866845B1 (en) | Lead-free piezoelectric ceramic composition with excellent electric field-induced strain property and preparation method of the same | |
| CN102503407A (en) | Lead-free X8R-type multilayer ceramic capacitor dielectric 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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200710 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |