CN116063072B - High-temperature piezoelectric ceramic heterojunction material and preparation method thereof - Google Patents
High-temperature piezoelectric ceramic heterojunction material and preparation method thereof Download PDFInfo
- Publication number
- CN116063072B CN116063072B CN202310076567.6A CN202310076567A CN116063072B CN 116063072 B CN116063072 B CN 116063072B CN 202310076567 A CN202310076567 A CN 202310076567A CN 116063072 B CN116063072 B CN 116063072B
- Authority
- CN
- China
- Prior art keywords
- piezoelectric ceramic
- layer
- temperature
- heterojunction material
- temperature piezoelectric
- 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
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
- C04B35/472—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 lead 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
- C04B35/638—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
- 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
- C04B41/5116—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
-
- 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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
-
- 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
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
-
- 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
Abstract
The invention discloses a high-temperature piezoelectric ceramic heterojunction material and a preparation method thereof, comprising the following steps: preparing a ceramic material with a bismuth layer structure on the layer A; preparing a ceramic material with a bismuth scandium acid-lead titanate structure as a layer B; mixing and pressing the A layer and the B layer according to a specific proportion according to at least one lamination mode in AB, ABA, BAB; and firing by adopting a specific plastic-arranging sintering process to form the high-temperature piezoelectric ceramic heterojunction material. The preparation method is low in preparation cost, and the prepared high-temperature piezoelectric ceramic heterojunction material has more practical use value.
Description
Technical Field
The invention belongs to the technical field of piezoelectric ceramic materials, and particularly relates to a high-temperature piezoelectric ceramic heterojunction material and a preparation method thereof.
Background
The high-temperature piezoelectric material is widely applied to a plurality of high-tech fields requiring to work under special environments, such as aerospace, geological exploration, petrochemical industry, automobile engines and the like, and the high-temperature piezoelectric material is needed to be used for a micro-displacement driver on a satellite, an automobile electronic injection, a vibration sensor, an acceleration sensor and the like in the geological exploration process. In recent years, the fields of automobile manufacturing, energy exploration, aerospace and the like rapidly develop, and strict conditions are put forward for the application environment of piezoelectric materials, such as an electronic injection device of an automobile internal combustion engine, so that the piezoelectric materials are required to stably work in a high-temperature environment of 200 ℃ or even more than 300 ℃; in the petroleum exploration process, a deep well detection oil pressure and other parameter pressure sensor also provides new challenges for piezoelectric materials; the detection of engine vibration conditions in the aerospace field requires that the piezoelectric material works at a higher temperature, and the application research of the piezoelectric material and devices thereof working in a severe environment has received unprecedented attention and importance.
The piezoelectric ceramic has the advantages of excellent piezoelectric performance, rich component adjustability, simple preparation process, low cost and the like, and always occupies most of market share of the piezoelectric material. The high-temperature piezoelectric ceramic material comprises a plurality of material systems such as niobate-based piezoelectric ceramic, bismuth-layer-structure piezoelectric ceramic, tungsten bronze-structure piezoelectric ceramic, lead titanate-based piezoelectric ceramic and the like. The most widely used piezoelectric materials at present are mainly lead titanate-based piezoelectric ceramic materials PZT, which have excellent piezoelectric properties. However, the curie temperature of the piezoelectric ceramic material is generally below 390 ℃, and the piezoelectric ceramic material cannot work normally above the curie temperature due to the depolarization phenomenon of the piezoelectric ceramic material. With the rapid development of industries such as aerospace and geological exploration, a required piezoelectric ceramic material often needs to work at 400 ℃ or higher, so that a piezoelectric ceramic material with high curie temperature and excellent piezoelectric performance is required to be required.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a high-temperature piezoelectric ceramic heterojunction material and a preparation method thereof. The technical problems to be solved by the invention are realized by the following technical scheme:
in a first aspect, an embodiment of the present invention provides a method for preparing a high temperature piezoelectric ceramic heterojunction material, including:
preparing a ceramic material with a bismuth layer structure on the layer A;
preparing a ceramic material with a bismuth scandium acid-lead titanate structure as a layer B;
mixing and pressing the A layer and the B layer according to a specific proportion according to at least one lamination mode in AB, ABA, BAB;
and firing by adopting a specific plastic-arranging sintering process to form the high-temperature piezoelectric ceramic heterojunction material.
In one embodiment of the present invention, preparing a ceramic material with a bismuth layer structure as a layer comprises:
proportioning according to the stoichiometric ratio of Na, bi, ti and Cr in the material composition, wherein the raw materials adopt Na 2 CO 3 Powder, bi 2 O 3 Powder, tiO 2 Powder and Cr 2 O 3 Powder;
the ingredients are gradually subjected to ball milling mixing, presintering, secondary ball milling, drying and grinding processes to prepare mixed powder;
adding the mixed powder obtained by the preparation into PVA (polyvinyl acetate) as an adhesive, and granulating to form a layer A.
In one embodiment of the invention, a ceramic material with a B layer of bismuth scandium acid and lead titanate structure is prepared, which comprises
According to the chemical composition of (1-x) BiScO 3 -xPbTiO 3 Is to weigh the Sc of the raw material 2 O 3 、Bi 2 O 3 、PbO、TiO 2 The method comprises the steps of carrying out a first treatment on the surface of the Wherein (1-x) and x each represent BiScO 3 、PbTiO 3 Molar ratio of (3);
gradually ball-milling and mixing the weighed raw materials, presintering, secondary ball-milling, drying and grinding to prepare mixed powder;
adding the mixed powder obtained by the preparation into PVA (polyvinyl acetate) as an adhesive, and granulating to form a layer B.
In one embodiment of the present invention, the a layer and the B layer are mixed and pressed in a specific ratio, comprising:
mixing the layer A and the layer B in a ratio of 1-3: mixing and pressing to form the product in the molar ratio of 1-3.
In one embodiment of the present invention, before firing to form the high temperature piezoelectric ceramic heterojunction material using the specific plastic-lined sintering process, the method further comprises:
the adhesive PVA in the A layer and the B layer is discharged at 600-600 ℃ respectively.
In one embodiment of the invention, firing with a specific plastic displacement sintering process forms a high temperature piezoelectric ceramic heterojunction material comprising:
and firing the high-temperature piezoelectric ceramic heterojunction material under the technological conditions that the plastic discharging temperature is 600-600 ℃, the sintering temperature is 1050-1150 ℃ and the sintering heat preservation time is 2-4 h.
In one embodiment of the present invention, further comprising:
electrodes are grown on the upper and lower surfaces of the high-temperature piezoelectric ceramic heterojunction material, and the related performance of the high-temperature piezoelectric ceramic heterojunction material is tested.
In one embodiment of the present invention, growing electrodes on upper and lower surfaces of a high temperature piezoelectric ceramic heterojunction material and testing the related properties of the high temperature piezoelectric ceramic heterojunction material comprises:
growing Ag electrodes on the upper and lower surfaces of the high-temperature piezoelectric ceramic heterojunction material under the process conditions that the silver burning temperature is 500-600 ℃ and the silver burning heat preservation time is 1-2 h;
and (3) carrying out direct-current high-voltage polarization under the polarization conditions that the polarization voltage is 6 kV/mm-8 kV/mm and the polarization time is 20 min-40 min in silicone oil with the temperature of 120-200 ℃, and carrying out the related performance on the high-temperature piezoelectric ceramic heterojunction material after the polarization.
In one embodiment of the present invention, before growing electrodes on the upper and lower surfaces of the high temperature piezoelectric ceramic heterojunction material, the method comprises:
polishing the upper and lower surfaces of the high-temperature piezoelectric ceramic heterojunction material.
In a second aspect, an embodiment of the present invention provides a high temperature piezoelectric ceramic heterojunction material, which is prepared according to any one of the preparation methods of the high temperature piezoelectric ceramic heterojunction material described above.
The invention has the beneficial effects that:
the preparation method of the high-temperature piezoelectric ceramic heterojunction material provided by the invention has the advantages that the ceramic material with the bismuth layer structure and the ceramic material with the bismuth scandium acid-lead titanate structure form the heterojunction, the dosage of Sc in the traditional single bismuth scandium acid-lead titanate structure is reduced, the manufacturing cost is reduced, and the prepared high-temperature piezoelectric ceramic heterojunction material keeps the Curie temperature T C Reaching a temperature of more than 500 ℃ and piezoelectric property d 33 The piezoelectric performance is improved by more than 3 times compared with a single bismuth layer-structured ceramic material and the Curie temperature T is improved by more than 100pC/N compared with a single bismuth scandium acid-lead titanate structure ceramic material C Can reach more than 500 ℃, has more market prospect in practical application, and can promote the development of high-temperature piezoelectric material research. Therefore, the embodiment of the invention has low preparation cost and simple process, is suitable for mass industrialized production, and promotes the development of the field of high-temperature piezoelectric ceramic materials.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of a high-temperature piezoelectric ceramic heterojunction material provided by an embodiment of the invention;
FIG. 2 is a schematic flow chart of another method for preparing a high-temperature piezoelectric ceramic heterojunction material according to an embodiment of the present invention;
fig. 3 is a schematic diagram showing performance comparison between a high-temperature piezoelectric ceramic heterojunction material and two other conventional piezoelectric ceramic materials according to an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but embodiments of the present invention are not limited thereto.
The existing piezoelectric ceramic material comprises a plurality of material systems such as niobate-based piezoelectric ceramic, bismuth-layer-structure piezoelectric ceramic, tungsten bronze-structure piezoelectric ceramic, lead titanate-based piezoelectric ceramic and the like, and the material of each system has the advantages of the material, such as high piezoelectric performance of some materials, high Curie temperature of some materials, and few materials with high piezoelectric performance and high Curie temperature. Most of the existing high-temperature piezoelectric ceramic materials are mainly researched by a single system, and the respective systems have corresponding defects, so that how to obtain the materials with high piezoelectric performance or high Curie temperature through the existing materials with high piezoelectric performance and high Curie temperature becomes a hot spot of the current research.
The inventor has found that the chemical general formula of the piezoelectric ceramic material (BLSF) with the bismuth layer structure is (Bi) 2 O 2 ) 2+ (A m-1 B m O 3m+1 ) 2- Is composed of a perovskite-like structure layer (A m-1 B m O 3m+1 ) 2- And bismuth oxide layer (Bi) 2 O 2 ) 2+ Is staggered in the direction of the c axis, wherein A is Bi + 、Ba 2+ 、Ca 2+ 、Sr 2+ 、K + 、Na + 、La 3+ Ion or complex ion suitable for 12 coordination, B is Nb 5+ 、Ta 5+ 、W 6+ 、Co 3+ And the number of layers corresponding to the perovskite structure between bismuth oxide layers is 1-5. In general, the larger the m value, the higher the piezoelectric performance of the BLSF piezoelectric ceramic material, but the lower the curie temperature. Based on the special layered structure, the bismuth layered structure piezoelectric ceramic material has the advantages of high Curie temperature, strong spontaneous polarization, obvious electrical property anisotropy, low dielectric constant, small dielectric loss, high mechanical quality factor, high resistivity, easy sintering and the like, but the spontaneous polarization steering is limited by a two-dimensional crystal structure, so that the piezoelectric property of the BLSF piezoelectric ceramic is very low, and the coercive field is very high, so that the material polarization is difficult. Research on piezoelectric ceramics with bismuth layered structure usually has Na with two-layer structure 0.5 Bi 2.5 Nb 2 O 9 、CaBi 2 Nb 2 O 9 Bi of three-layer structure 4 Ti 3 O 12 And CaBi of a four-layer structure 4 Ti 4 O 15 、Na 0.5 Bi 4.5 Ti 4 O 15 、K 0.5 Bi 4.5 Ti 4 O 15 、SrBi 4 Ti 4 O 15 Etc., piezoelectric property d 33 At about 15pC/N to 30pC/N with Curie temperature T C Above 550 ℃, the piezoelectric performance is relatively low, but the piezoelectric ceramic has the advantages of small dielectric loss, high mechanical quality factor, high resistivity, good temperature stability and the like, and is suitable for the design and application of piezoelectric sensors in the field of high-temperature piezoelectric, such as high-temperature acceleration sensors and the like.
It has also been found by the inventors that lead titanate (PbTiO) 3 PT) piezoelectric ceramic material has a curie temperature of 490 ℃, but is difficult to sinter, mainly because c/a is relatively large in a tetragonal phase structure, and the ceramic material is easy to crack due to overlarge stress in a cubic phase-to-tetragonal phase transformation process occurring near the curie temperature in a sintering cooling process. Meanwhile, the c/a is large, so that the coercive field of the material is large, polarization is difficult, and the lead titanate piezoelectric ceramic material has a high Curie temperature, but has poor piezoelectric performance, and is difficult to be put into practical use. In 2001 Eitel et al reported a bismuth-based high temperature piezoelectric ceramic system of the general formula Bi (Me) O 3 -PbTiO 3 Wherein Me represents an ion of the +3 valence state or an ionic group, e.g. Sc +3 、In +3 、Yb +3 And the like, the system not only has excellent piezoelectric performance at the quasi-homotype phase boundary (Morphotropic Phase Boundary, MPB for short) component, but also maintains higher Curie temperature, and is widely focused by researchers, wherein BiScO is adopted 3 -PbTiO 3 The (hereinafter abbreviated as BS-PT) piezoelectric ceramic material is attracting attention. BS-PT is a binary solid solution with a perovskite structure, and the piezoelectric property d of the material is about 64mol% of PT in the MPB component 33 Up to 460pC/N with Curie temperature T C The temperature is kept at about 450 ℃, and the price of Sc element in the BS-PT-based piezoelectric ceramic restricts the large-scale industrial production to a certain extent, but the BS-PT-based piezoelectric ceramic still receives close attention of vast researchers in the field of high-temperature piezoelectric ceramic, especially in the aspect of application research of aerospace.
Based on the research and analysis of the BLSF and BS-PT materials, a single BLSF and a single BS-PT material respectively have the applicable scenes,for other scenes beyond the applicable scenes, the advantages of the single BLSF and BS-PT materials are not highlighted any more, and the single BLSF and BS-PT materials are the important factors for restricting the development of the single BLSF and BS-PT materials in other fields of high-temperature piezoelectric ceramic materials. Such as bismuth sodium titanate (Na) 0.5 Bi 4.5 Ti 4 O 15 ) Is a BLSF material with m=4, curie temperature as high as 656 ℃, piezoelectric property d 33 About 16pC/N, dielectric loss tan delta<0.5%, compared with the actual application, although the Curie temperature T C >550 ℃ meets the requirement of high-temperature use, but the piezoelectric performance of the piezoelectric ceramic cannot meet the application requirement, such as d 33 >30 pC/N. The invention provides a preparation method of a high-temperature piezoelectric ceramic heterojunction material based on BLSF and BS-PT materials, which combines the advantages of two material systems, and the prepared high-temperature piezoelectric ceramic material can promote the development of the field of high-temperature piezoelectric ceramic materials. Referring specifically to fig. 1, the embodiment of the invention provides a preparation method of a high-temperature piezoelectric ceramic heterojunction material, which comprises the following steps:
s10, preparing a ceramic material with a bismuth layer structure in the layer A.
The embodiment of the invention provides an alternative scheme for preparing a ceramic material with a bismuth layer structure, which comprises the following steps: proportioning according to the stoichiometric ratio of Na, bi, ti and Cr in the material composition, wherein the raw materials adopt Na 2 CO 3 Powder, bi 2 O 3 Powder, tiO 2 Powder and Cr 2 O 3 The purity of the powder is analytically pure, and the powder can be directly purchased from the market;
the ingredients are gradually subjected to the processes of ball milling mixing, presintering, secondary ball milling, drying, grinding and the like to prepare mixed powder; wherein, the ball milling time of the ball milling tank is 18 hours, the ball milling medium is absolute ethyl alcohol, the presintering temperature is 600-900 ℃, and the presintering heat preservation time is 2-4 hours.
Adding the mixed powder obtained by the preparation method into adhesive PVA (polyvinyl alcohol) and granulating to form a layer A, namely the ceramic material BLSF with the bismuth lamellar structure.
S20, preparing a ceramic material with a B layer in a bismuth scandium acid-lead titanate structure.
The embodiment of the invention provides an alternative scheme for preparing a ceramic material with a B layer of bismuth scandium acid and lead titanate structure, which comprises the following steps: according to the chemical composition of (1-x) BiScO 3 -xPbTiO 3 Is to weigh the Sc of the raw material 2 O 3 、Bi 2 O 3 、PbO、TiO 2 The method comprises the steps of carrying out a first treatment on the surface of the Wherein (1-x) and x each represent BiScO 3 、PbTiO 3 Molar ratio of (3);
the weighed raw materials are subjected to ball milling mixing, presintering, secondary ball milling, drying, grinding and other processes step by step to prepare mixed powder; wherein, the ball milling time of the ball milling tank is 18 hours, the ball milling medium is absolute ethyl alcohol, the presintering temperature is 600-900 ℃, and the presintering heat preservation time is 2-4 hours.
Adding the prepared mixed powder into a binding agent PVA, and granulating to form a B layer, namely the bismuth scandium acid-lead titanate structured ceramic material BS-PT.
S30, mixing and pressing the A layer and the B layer according to a specific proportion according to at least one lamination mode in AB, ABA, BAB.
According to the embodiment of the invention, a lamination mode of two materials of the layer A and the layer B comprises AB, ABA, BAB, a heterojunction is formed between the adjacent layer A and the adjacent layer B, and in the heterojunction forming process of the layer A and the layer B, the layer A and the layer B are required to meet the specific molar ratio, and the mixed compression molding can simultaneously have the advantages of high piezoelectric performance or high Curie temperature, and the inventor researches: mixing the layer A and the layer B in a ratio of 1-3: 1-3, and applying 300MPa pressure by a tablet press, and the other proportion mixing pressing can have the advantages of high piezoelectric performance or high Curie temperature.
If the AB is a lamination mode, the A layer and the B layer can be mixed and pressed according to any mole ratio of 1:1, 1:2, 1:3, 2:1, 2:2, 2:3, 3:1, 3:2 and 3:3; other ABA, BAB layering approaches are similar and will not be described in detail here.
And S40, firing by adopting a specific plastic-arranging sintering process to form the high-temperature piezoelectric ceramic heterojunction material.
The embodiment of the invention further comprises the following steps before the high-temperature piezoelectric ceramic heterojunction material is formed by firing by adopting a specific plastic-arranging sintering process: the adhesive PVA in the A layer and the B layer is discharged at 600-600 ℃ respectively.
Next, an alternative scheme is provided in the embodiments of the present invention, in which a specific plastic-displacement sintering process is used for firing to form a high-temperature piezoelectric ceramic heterojunction material, including: and firing the high-temperature piezoelectric ceramic heterojunction material under the technological conditions that the plastic discharging temperature is 600-600 ℃, the sintering temperature is 1050-1150 ℃ and the sintering heat preservation time is 2-4 h. In the experimental process, when the selection of the plastic-discharging sintering process conditions for forming the heterojunction between the layer A and the layer B is inappropriate, a heterojunction structure cannot be formed between the layer A and the layer B, and through multiple experiments, the high-temperature piezoelectric ceramic material with the heterojunction structure can be formed by sintering under the process conditions that the plastic-discharging temperature is 600-600 ℃, the sintering temperature is 1050-1150 ℃ and the sintering heat preservation time is 2-4 hours.
Further, referring to fig. 2, the method for preparing the high-temperature piezoelectric ceramic heterojunction material according to the embodiment of the invention further includes:
and S50, growing electrodes on the upper surface and the lower surface of the high-temperature piezoelectric ceramic heterojunction material, and testing the related performance of the high-temperature piezoelectric ceramic heterojunction material.
The embodiment of the invention comprises the following steps before electrodes grow on the upper surface and the lower surface of a high-temperature piezoelectric ceramic heterojunction material: polishing the upper and lower surfaces of the high-temperature piezoelectric ceramic heterojunction material, wherein the polishing can be performed by removing the upper and lower surfaces of the high-temperature piezoelectric ceramic heterojunction material with a preset thickness, such as 0.4mm thickness, so as to remove the influence of surface defects.
Next, an alternative solution is provided in the embodiments of the present invention, in which electrodes are grown on the upper and lower surfaces of the high temperature piezoelectric ceramic heterojunction material after polishing treatment, and the related properties of the high temperature piezoelectric ceramic heterojunction material are tested, including:
growing Ag electrodes on the upper and lower surfaces of the high-temperature piezoelectric ceramic heterojunction material under the process conditions that the silver burning temperature is 500-600 ℃ and the silver burning heat preservation time is 1-2 h;
after silver burning treatment, the silicon oil with the silicon oil temperature of 120-200 ℃ is subjected to direct-current high-voltage polarization under the polarization conditions of the polarization voltage of 6-8 kV/mm and the polarization time of 20-40 min, and the related properties of the polarized high-temperature piezoelectric ceramic heterojunction material, including Curie temperature, piezoelectric property, dielectric loss and the like, are added.
Through testing, the high-temperature piezoelectric ceramic heterojunction material prepared by the embodiment of the invention has Curie temperature T C At a temperature of 500 ℃ or higher, the piezoelectric property d 33 Up to 108pC/N, and has good high temperature stability, dielectric loss tan delta is still lower than 0.2% at more than 500 ℃, and has good application prospect in the high temperature field.
In order to verify the effectiveness of the preparation method of the high-temperature piezoelectric ceramic heterojunction material provided by the embodiment of the invention, the following experiment is carried out for verification.
The experimental process of the embodiment of the invention comprises the following steps: preparing a ceramic material BLSF with a bismuth layered structure and a ceramic material BS-PT with a bismuth scandium acid-lead titanate structure respectively; respectively adding adhesive polyvinyl alcohol PVA for granulating; the prepared ceramic material BLSF with the bismuth layer structure and the ceramic material BS-PT with the bismuth scandium acid-lead titanate structure form heterojunction, wherein the composition ratio comprises 1:1, 1:2 and 1:3; placing the obtained heterojunction into a die, and pressing the heterojunction by using a tablet press under 300 MPa; discharging adhesive polyvinyl alcohol PVA in the heterojunction material at 600-600 ℃; firing for 3 hours at the plastic discharging temperature of about 650 ℃ and about 1100 ℃ to form a high-temperature piezoelectric ceramic heterojunction material with the diameter of 10 mm; and covering the surface of the sintered high-temperature piezoelectric ceramic heterojunction material with a silver electrode, polarizing for 20min at a voltage of 6kV/mm, and testing the performance after aging for 24 h.
The embodiment of the invention compares the traditional single bismuth layer-structured ceramic material BLSF, the traditional single bismuth scandium acid-lead titanate structured ceramic material BS-PT and the high-temperature piezoelectric ceramic heterojunction material prepared by the experimental process, and the comparison result is shown in figure 3, and the single BLSF and BS-PT only have higher piezoelectric property d 33 Or Curie temperature T C The high-temperature piezoelectric ceramic heterojunction material prepared by the embodiment of the invention maintains the piezoelectric property d 33 And Curie temperature T C All are more in one practical applicationIn the range of the demand, the method has practical use value and market prospect.
In summary, the embodiment of the invention provides a method for preparing a high-temperature piezoelectric ceramic heterojunction material, which comprises a heterojunction composed of a bismuth layer-structured ceramic material and a bismuth scandium acid-lead titanate-structured ceramic material, so that the amount of Sc in the traditional single bismuth scandium acid-lead titanate-structured ceramic heterojunction material is reduced, the manufacturing cost is reduced, and the prepared high-temperature piezoelectric ceramic heterojunction material maintains the Curie temperature T C Reaching a temperature of more than 500 ℃ and piezoelectric property d 33 The piezoelectric performance is improved by more than 3 times compared with a single bismuth layer-structured ceramic material and the Curie temperature T is improved by more than 100pC/N compared with a single bismuth scandium acid-lead titanate structure ceramic material C Can reach more than 500 ℃, has more market prospect in practical application, and can promote the development of high-temperature piezoelectric material research. Therefore, the embodiment of the invention has low preparation cost and simple process, is suitable for mass industrialized production, and promotes the development of the field of high-temperature piezoelectric ceramic materials.
In a second aspect, an embodiment of the present invention provides a high temperature piezoelectric ceramic heterojunction material, which is prepared by using the preparation method of any one of the high temperature piezoelectric ceramic heterojunction materials according to the first aspect. For the material embodiments of the second aspect, the description is relatively simple as it is substantially similar to the preparation method embodiments of the first aspect, and the relevant points are referred to in the description of the preparation method embodiments of the first aspect.
In the description of the present invention, it should be understood that the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
Although the invention is described herein in connection with various embodiments, other variations to the disclosed embodiments can be understood and effected by those skilled in the art in practicing the claimed invention, from a study of the specification and the drawings. In the description, the word "comprising" does not exclude other elements or steps, and the "a" or "an" does not exclude a plurality. Some measures are described in mutually different embodiments, but this does not mean that these measures cannot be combined to produce a good effect.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (6)
1. The preparation method of the high-temperature piezoelectric ceramic heterojunction material is characterized by comprising the following steps of:
preparing a ceramic material with a bismuth layer structure on the layer A;
preparing a ceramic material with a bismuth scandium acid-lead titanate structure as a layer B;
mixing and pressing the A layer and the B layer according to a specific proportion according to at least one lamination mode in AB, ABA, BAB;
firing by adopting a specific plastic-arranging sintering process to form a high-temperature piezoelectric ceramic heterojunction material;
wherein, preparing the ceramic material with the A layer of bismuth layer structure comprises:
proportioning according to the stoichiometric ratio of Na, bi, ti and Cr in the material composition, wherein the raw materials adopt Na 2 CO 3 Powder, bi 2 O 3 Powder, tiO 2 Powder and Cr 2 O 3 Powder;
the ingredients are gradually subjected to ball milling mixing, presintering, secondary ball milling, drying and grinding processes to prepare mixed powder;
adding the adhesive PVA into the prepared mixed powder, and granulating to form a layer A;
the preparation method of the ceramic material with the B layer of the bismuth scandium acid-lead titanate structure comprises the following steps:
according to the chemical composition of (1)x)BiScO 3 -xPbTiO 3 Is to weigh the Sc of the raw material 2 O 3 、Bi 2 O 3 、PbO、TiO 2 The method comprises the steps of carrying out a first treatment on the surface of the Wherein (1-x) Andxrespectively represent BiScO 3 、PbTiO 3 Molar ratio of (3);
gradually ball-milling and mixing the weighed raw materials, presintering, secondary ball-milling, drying and grinding to prepare mixed powder;
adding the adhesive PVA into the prepared mixed powder, and granulating to form a layer B;
mixing and pressing the layer A and the layer B according to a specific proportion, and forming the mixture, wherein the method comprises the following steps:
and mixing the layer A and the layer B by 1-3: mixing and pressing to form the mixture according to the molar ratio of 1-3;
the high-temperature piezoelectric ceramic heterojunction material is formed by firing by adopting a specific plastic-arranging sintering process, which comprises the following steps:
and firing under the process conditions that the plastic discharging temperature is 600-700 ℃, the sintering temperature is 1050-1150 ℃ and the sintering heat preservation time is 2-4 hours to form the high-temperature piezoelectric ceramic heterojunction material.
2. The method of manufacturing a high temperature piezoelectric ceramic heterojunction material according to claim 1, further comprising, before firing with a specific plastic-displacement sintering process to form the high temperature piezoelectric ceramic heterojunction material:
and respectively discharging the adhesive PVA in the layer A and the layer B at 600-700 ℃.
3. The method of preparing a high temperature piezoelectric ceramic heterojunction material of claim 1, further comprising:
electrodes are grown on the upper and lower surfaces of the high-temperature piezoelectric ceramic heterojunction material, and the related performance of the high-temperature piezoelectric ceramic heterojunction material is tested.
4. The method for preparing a high temperature piezoelectric ceramic heterojunction material as claimed in claim 3, wherein growing electrodes on the upper and lower surfaces of the high temperature piezoelectric ceramic heterojunction material and testing the related properties of the high temperature piezoelectric ceramic heterojunction material comprises:
growing Ag electrodes on the upper and lower surfaces of the high-temperature piezoelectric ceramic heterojunction material under the process conditions that the silver burning temperature is 500-600 ℃ and the silver burning heat preservation time is 1-2 hours;
and (3) carrying out direct-current high-voltage polarization under the polarization condition that the polarization voltage is 6 kV/mm-8 kV/mm and the polarization time is 20 min-40 min in the silicone oil with the silicone oil temperature of 120-200 ℃, and carrying out the related performance on the high-temperature piezoelectric ceramic heterojunction material after the polarization.
5. The method for preparing a high temperature piezoelectric ceramic heterojunction material according to claim 3, wherein before growing electrodes on the upper and lower surfaces of the high temperature piezoelectric ceramic heterojunction material, comprising:
polishing the upper and lower surfaces of the high-temperature piezoelectric ceramic heterojunction material.
6. The high-temperature piezoelectric ceramic heterojunction material is characterized by being prepared by a preparation method of the high-temperature piezoelectric ceramic heterojunction material according to any one of claims 1-5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310076567.6A CN116063072B (en) | 2023-01-16 | 2023-01-16 | High-temperature piezoelectric ceramic heterojunction material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310076567.6A CN116063072B (en) | 2023-01-16 | 2023-01-16 | High-temperature piezoelectric ceramic heterojunction material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116063072A CN116063072A (en) | 2023-05-05 |
| CN116063072B true CN116063072B (en) | 2023-09-22 |
Family
ID=86169485
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310076567.6A Active CN116063072B (en) | 2023-01-16 | 2023-01-16 | High-temperature piezoelectric ceramic heterojunction material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116063072B (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1447452A (en) * | 2002-03-25 | 2003-10-08 | 株式会社村田制作所 | Piezoelectric component and its mfg. method |
| CN101346828A (en) * | 2005-12-26 | 2009-01-14 | 株式会社村田制作所 | Piezoelectric ceramic, process for producing said piezoelectric ceramic, piezoelectric resonator, and process for producing piezoelectric resonator |
| CN101552319A (en) * | 2008-03-31 | 2009-10-07 | 株式会社电装 | Method of producing a piezostack device |
| CN101973764A (en) * | 2010-10-15 | 2011-02-16 | 同济大学 | Textured calcium bismuth niobate ceramic material and preparation method thereof |
| CN203521478U (en) * | 2013-09-26 | 2014-04-02 | 北京科技大学 | Ferroelectric/ferromagnetic superlattice structure and memory thereof |
| CN105622094A (en) * | 2014-10-28 | 2016-06-01 | 铜仁学院 | Preparation method of high-electrical-resistivity high-temperature piezoelectric ceramic material |
| CN106631007A (en) * | 2016-12-13 | 2017-05-10 | 成都大学 | High-temperature high-performance high-stability bismuth laminated-structure piezoelectric ceramic material and application thereof |
| CN107759219A (en) * | 2017-11-14 | 2018-03-06 | 广州光鼎科技有限公司 | A kind of high curie temperature leadless piezoelectric ceramal and preparation method thereof |
| EP3409652A1 (en) * | 2017-05-31 | 2018-12-05 | Consejo Superior de Investigaciones Cientificas (CSIC) | A high temperature and voltage response piezoelectric, bisco3-pbtio3 based ceramic material microstructurally engineered for enhanced mechanical performance, a procedure for obtaining said ceramic material and its use as sensing device |
| CN113213918A (en) * | 2021-06-25 | 2021-08-06 | 济南大学 | Strontium bismuth titanate-bismuth scandium acid-lead titanate series high-temperature piezoelectric ceramic material with high piezoelectric performance and low loss and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4567768B2 (en) * | 2008-05-30 | 2010-10-20 | 株式会社デンソー | Manufacturing method of multilayer piezoelectric element |
-
2023
- 2023-01-16 CN CN202310076567.6A patent/CN116063072B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1447452A (en) * | 2002-03-25 | 2003-10-08 | 株式会社村田制作所 | Piezoelectric component and its mfg. method |
| CN101346828A (en) * | 2005-12-26 | 2009-01-14 | 株式会社村田制作所 | Piezoelectric ceramic, process for producing said piezoelectric ceramic, piezoelectric resonator, and process for producing piezoelectric resonator |
| CN101552319A (en) * | 2008-03-31 | 2009-10-07 | 株式会社电装 | Method of producing a piezostack device |
| CN101973764A (en) * | 2010-10-15 | 2011-02-16 | 同济大学 | Textured calcium bismuth niobate ceramic material and preparation method thereof |
| CN203521478U (en) * | 2013-09-26 | 2014-04-02 | 北京科技大学 | Ferroelectric/ferromagnetic superlattice structure and memory thereof |
| CN105622094A (en) * | 2014-10-28 | 2016-06-01 | 铜仁学院 | Preparation method of high-electrical-resistivity high-temperature piezoelectric ceramic material |
| CN106631007A (en) * | 2016-12-13 | 2017-05-10 | 成都大学 | High-temperature high-performance high-stability bismuth laminated-structure piezoelectric ceramic material and application thereof |
| EP3409652A1 (en) * | 2017-05-31 | 2018-12-05 | Consejo Superior de Investigaciones Cientificas (CSIC) | A high temperature and voltage response piezoelectric, bisco3-pbtio3 based ceramic material microstructurally engineered for enhanced mechanical performance, a procedure for obtaining said ceramic material and its use as sensing device |
| CN107759219A (en) * | 2017-11-14 | 2018-03-06 | 广州光鼎科技有限公司 | A kind of high curie temperature leadless piezoelectric ceramal and preparation method thereof |
| CN113213918A (en) * | 2021-06-25 | 2021-08-06 | 济南大学 | Strontium bismuth titanate-bismuth scandium acid-lead titanate series high-temperature piezoelectric ceramic material with high piezoelectric performance and low loss and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116063072A (en) | 2023-05-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhao et al. | Giant piezoelectricity of ternary perovskite ceramics at high temperatures | |
| Haertling | Ferroelectric ceramics: history and technology | |
| EP1875526B1 (en) | Compositions for high power piezoelectric ceramics | |
| US10217566B2 (en) | Ceramic material and capacitor comprising the ceramic material | |
| Ning et al. | Achieving both large piezoelectric constant and high Curie temperature in BiFeO3-PbTiO3-BaTiO3 solid solution | |
| CN106554202B (en) | A kind of bismuth laminated bismuth-sodium titanate high temperature piezoceramics and preparation method thereof | |
| CN102850050B (en) | Low temperature sintering piezoelectric ceramic material and preparation method thereof | |
| WO2011111643A1 (en) | Piezoelectric material and devices using the same | |
| CN102272962A (en) | Piezoelectric material | |
| CN103172374A (en) | Piezoelectric ceramic and piezoelectric device | |
| US20120112607A1 (en) | Ceramic composition for piezoelectric actuator and piezoelectric actuator including the same | |
| EP2948417A1 (en) | Lead-free piezoelectric material | |
| CN116063072B (en) | High-temperature piezoelectric ceramic heterojunction material and preparation method thereof | |
| GB2550887A (en) | Temperature stable lead-free piezoelectric/electrostrictive materials with enhanced fatigue resistance | |
| CN113213918A (en) | Strontium bismuth titanate-bismuth scandium acid-lead titanate series high-temperature piezoelectric ceramic material with high piezoelectric performance and low loss and preparation method thereof | |
| KR101099980B1 (en) | Lead-free piezoelectric ceramic composition | |
| CN115385675B (en) | Bismuth ferrite based lead-free ferroelectric ceramic material with high Curie temperature and energy storage characteristic and preparation method thereof | |
| JP4535721B2 (en) | Piezoelectric ceramic, multilayer piezoelectric element, and injection device | |
| US20120091861A1 (en) | Ceramic composition for piezoelectric actuator and piezoelectric actuator comprising the same | |
| CN113248247A (en) | Ternary piezoelectric ceramic and preparation method and application thereof | |
| JP2001284668A (en) | Laminated piezoelectric element, piezoelectric actuator, and injection equipment | |
| Li et al. | A new Pb (Lu1/2Nb1/2) O3–PbZrO3–PbTiO3 ternary solid solution with morphotropic region and high Curie temperature | |
| Takenaka | Bismuth-based piezoelectric ceramics | |
| Yoon et al. | Effect of Pb (Yb 1/2 Nb 1/2) O 3 on structural and piezoelectric properties of Pb (Zr 0.52 Ti 0.48) O 3 ceramics | |
| CN115490514B (en) | Piezoelectric ceramic and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |