CN109467428A - A kind of Ti Cu/W codope bismuth titanates high temperature piezoceramics and preparation method thereof - Google Patents

A kind of Ti Cu/W codope bismuth titanates high temperature piezoceramics and preparation method thereof Download PDF

Info

Publication number
CN109467428A
CN109467428A CN201910009551.7A CN201910009551A CN109467428A CN 109467428 A CN109467428 A CN 109467428A CN 201910009551 A CN201910009551 A CN 201910009551A CN 109467428 A CN109467428 A CN 109467428A
Authority
CN
China
Prior art keywords
powder
hours
temperature
ball milling
high temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910009551.7A
Other languages
Chinese (zh)
Inventor
郑鹏
李旭东
张栋格
陈振宁
盛林生
白王峰
郑梁
张阳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hangzhou Dianzi University
Hangzhou Electronic Science and Technology University
Original Assignee
Hangzhou Electronic Science and Technology University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hangzhou Electronic Science and Technology University filed Critical Hangzhou Electronic Science and Technology University
Priority to CN201910009551.7A priority Critical patent/CN109467428A/en
Publication of CN109467428A publication Critical patent/CN109467428A/en
Pending legal-status Critical Current

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
    • C04B35/475—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 bismuth 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
    • 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
    • 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
    • C04B41/45—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
    • C04B2235/3231—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
    • C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
    • 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)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses a kind of Ti Cu/W codope bismuth titanates high temperature piezoceramics and preparation method thereof, the general formula of the piezoceramic material is Bi4Ti3‑x(Cu1/2W1/2)xO12, wherein 0 < x≤0.04.The invention also discloses the preparation methods of the piezoceramic material, using Bi4Ti3O12Based on system piezoelectric material, a certain proportion of Cu, W are mixed in the Ti molar ratios according to 1:1, such novel laminated structure bismuth piezoelectric ceramic material is prepared using traditional solid phase synthesis process.Compared with prior art, the piezoceramic material that the present invention obtains, Specifeca tion speeification d33=34pC/N, TC=680 DEG C, at 500 DEG C, ρ=1.52 × 106Ω cm, furthermore stable preparation process is reliable, and production cost is low, it is easy to accomplish industrialized production has a good application prospect in high-temperature field.Using ceramic component made from this material, various piezoelectric transducers are assembled into, can be used under the special hot environment such as space flight and aviation, petrochemical industry.

Description

A kind of Ti Cu/W codope bismuth titanates high temperature piezoceramics and preparation method thereof
Technical field
The present invention relates to a kind of bismuth laminated bismuth titanates high temperature piezoceramics and preparation method thereof, and in particular to one Bismuth laminated bismuth titanates (the Bi of kind Cu/W codope4Ti3O12) piezoceramic material and its preparation, belong to piezoceramic material Field.
Background technique
Currently, most widely used piezoelectric material is mainly the PZT base piezoelectric ceramic of perovskite structure, but this kind of piezoelectricity is made pottery The Curie temperature of porcelain generally at 390 DEG C hereinafter, due to piezoelectric material depolarization phenomenon presence, piezoelectric material Curie temperature with Under can not work normally.With the rapid development of the industry such as aerospace, geological prospecting and the need of human social It asks, it is therefore necessary to seek a kind of Curie temperature height, the excellent environmentally friendly piezoelectric material of piezoelectric property.
Since Curie temperature is high, fatigue performance is good, bismuth laminated ceramics are considered as the reason of high-temperature piezoelectric material Want to select.Bismuth laminated ceramic material is by (Bi2O2)2+The lattice layer of layer and perovskite structure, which alternates, to be formed by stacking , chemical general formula is (Bi2O2)2+(Am-1BmO3m+1)2-, A is the ion for being suitble to dodecahedron coordination, such as Na in above formula+, Ca2+, La3+It is the ion for being suitble to octahedral coordination, such as Ti Deng, B4+, Nb5+, Ta5+Deng, m is integer, value be 1 to 6.Bismuth titanates (Bi4Ti3O12) be m=3 bismuth layer structure, Curie temperature is up to 675 DEG C, piezoelectric constant d33About 8pC/N, with reality Border is using comparing, although Curie temperature meets the requirement under high temperature, application requirement (d is not achieved in its piezoelectric property33> 30pC/N).In addition, the lower resistivity of bismuth titanate ceramics is also an important factor for limiting the application of its high temperature.Therefore, how not Piezoelectric property and resistivity are improved while reducing Curie temperature is made pottery with obtaining the bismuth layered piezoelectric stablized in high temperature range and used Ceramic material becomes an important topic of piezoceramic material area research.
Currently, there is not yet improving bismuth laminated bismuth titanates (Bi with Cu/W codope4Ti3O12) piezoceramic material The relevant report of energy.
Summary of the invention
Insufficient for the above-mentioned prior art, the object of the present invention is to provide a kind of Ti Cu/W codope bismuth titanates high-temperature high-pressures Electroceramics material and preparation method thereof, using Cu, W element to bismuth laminated bismuth titanates (Bi4Ti3O12) piezoceramic material into Row is codoping modified, while not reducing Curie temperature temperature, improves its piezoelectric property and resistivity, prepares a kind of novel , environmentally friendly piezoceramic material.
In order to overcome the shortcomings of the prior art, the present invention the following technical schemes are provided:
A kind of Ti Cu/W codope bismuth titanates high temperature piezoceramics, the general formula of the piezoceramic material are Bi4Ti3-x(Cu1/2W1/2)xO12, wherein 0 < x≤0.04；
In general formula, the molar ratio of index number representative element；
Preferred x=0.005,0.01,0.015,0.02,0.03 or 0.04；
It is further preferred that x=0.015；
The invention also discloses a kind of preparation method of Ti Cu/W codope bismuth titanates high temperature piezoceramics, steps It is as follows:
Ingredient: with Bi2O3Powder, TiO2Powder, CuO powder and WO3Powder is raw material, by Formula B i4Ti3-x(Cu1/ 2W1/2)xO12The stoichiometry of middle Bi, Ti, Cu and W carry out ingredient, wherein 0 < x≤0.04；
Ball milling: the dehydrated alcohol with mixture equivalent being added into said mixture, continues ball milling 12~24 hours, It is uniformly mixed powder and forms slurry, it is possible thereby to further improve the comprehensive performance of bismuth titanates high temperature piezoceramics；
Drying: above-mentioned slurry being placed in constant temperature oven and is toasted, and is removed dehydrated alcohol, and grind in mortar, is obtained powder Material；
Tabletting pre-burning: powder being placed in grinding tool and is pressed into material block in advance, will expect block pre-burning, and calcined temperature is 675~750 DEG C, Soaking time 2~4 hours；
Secondary ball milling: by the material block after pre-burning in mortar, primary powder is obtained after being pulverized grinding, to obtained primary The dehydrated alcohol with primary powder equivalent is added in powder, continues ball milling 12~24 hours, is uniformly mixed powder and forms slurry；
Drying: above-mentioned slurry being placed in constant temperature oven and is toasted, and removes dehydrated alcohol, and powder is ground into mortar；
Granulating and forming: the poly-vinyl alcohol solution (PVA) that distilled water and concentration are 8% is mixed into powder as adhesive In, the quality of the distilled water of incorporation is the 2.5% of powder quality, and the quality of the adhesive of incorporation is the 5% of powder quality, is being ground It is uniformly mixed in alms bowl；Mixed powder is placed in grinding tool, green compact are pressed into；Green compact are milled to powder in mortar, are led to The sieve for crossing 60 mesh and 120 mesh takes the powder of 60 mesh and 120 mesh sieve middle layers, has obtained the suitable powder of granular size Material；Powder is placed in grinding tool, is pressed into green compact under the pressure of 200MPa；
Dumping: green compact dumping was excluded the PVA in green compact, obtains porcelain billet temperature lower calcination 3 hours of 650 DEG C；
Sintering: porcelain billet is sintered, and sintering temperature is 1000~1100 DEG C, soaking time 2~4 hours, obtains ceramics Piece；
It applies electrode: potsherd cleaning, drying, screen printing being brushed into silver electrode, silver ink firing, 500~600 DEG C of silver ink firing temperature, protected 1~2 hour warm time；
Polarization: the potsherd for having plated silver electrode is placed in 120~160 DEG C of silicone oil, polarizing voltage be 12kV/mm~ 15kV/mm, polarization time are 20min~40min.
Preferably, during a ball milling and secondary ball milling, the Ball-milling Time is 12 hours.
Preferably, in the burn-in process, the calcined temperature is 675 DEG C, and the soaking time is 4 hours.
Preferably, in the sintering process, the sintering temperature is 1050 DEG C, and the soaking time is 4 hours.
Compared with prior art, technical solution of the present invention, B Ti are replaced by Cu and W, and control doped chemical Additional amount, effectively increase the piezoelectric property of bismuth titanates high temperature piezoceramics, and obtain higher resistivity.It needs Illustrate, although being different in the prior art there are many about the report for carrying out element doping to piezoceramic material Doped chemical, the different additional amount of doped chemical can all produce bigger effect the overall performance of piezoceramic material, then need Constantly grope during the test, repetition test can just obtain, and inventor has also attempted a variety of different elements in early-stage study Doping to bismuth titanates high temperature piezoceramics, but the doping for other elements are co-doped with using Cu and W element of the invention Miscellaneous, the bismuth laminated bismuth titanates high-temperature piezoelectric material being prepared shows more excellent piezoelectric property and resistivity.
It is excellent that experimental data shows that the present invention has the effect of:
The codoping modified bismuth layered titanic acid bismuth (Bi of Cu, W element of the present invention4Ti3O12) piezoceramic material, Curie temperature It is 680 DEG C, piezoelectric constant d33Up to 34pC/N, and there is good high-temperature stability, at 500 DEG C, electricalresistivityρ=1.52 × 106Ω cm has a good application prospect in high-temperature field.
In addition, the invention is made by conventional piezoelectric ceramic industry, preparation cost is low, and industry is simple and is suitable for high-volume The piezoelectric property of industrialized production, the ceramic material after doping vario-property improves four times or more than before, advances high-temperature piezoelectric The progress of material.
Detailed description of the invention
Fig. 1 is the Bi prepared in embodiment 14Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction pattern of x=0.005 ceramics, and The curve of dielectric constant with temperature variation；
Fig. 2 is the Bi prepared in embodiment 24Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction pattern of x=0.01 ceramics, Yi Jijie The curve that electric constant varies with temperature；
Fig. 3 is the Bi prepared in embodiment 34Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction pattern of x=0.015 ceramics, and The curve of dielectric constant with temperature variation；
Fig. 4 is the Bi prepared in embodiment 44Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction pattern of x=0.02 ceramics, Yi Jijie The curve that electric constant varies with temperature；
Fig. 5 is the Bi prepared in embodiment 54Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction pattern of x=0.03 ceramics, Yi Jijie The curve that electric constant varies with temperature；
Fig. 6 is the Bi prepared in embodiment 64Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction pattern of x=0.04 ceramics, Yi Jijie The curve that electric constant varies with temperature；
Fig. 7 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12The Curie temperature variation diagram of ceramics；
Fig. 8 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12The room temperature piezoelectric modulus variation diagram of ceramics；
Fig. 9 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics 500 DEG C when change in resistance figure.
Specific embodiment
The present invention will be further explained with reference to the examples below.
Embodiment 1
Preparation meets chemical composition Bi4Ti3-x(Cu1/2W1/2)xO12, the Cu/W of x=0.005 codoping modified bismuth titanates (Bi4Ti3O12) leadless piezoelectric ceramics, including the following steps:
(1) ingredient: with Bi2O3Powder, TiO2Powder, CuO powder and WO3Powder is raw material, by Bi, Ti, Cu in general formula and The stoichiometry of W carries out ingredient；
(2) ball millings: the dehydrated alcohol with mixture equivalent being added into said mixture, continues ball milling 12 hours, It is uniformly mixed powder and forms slurry, it is possible thereby to further improve the comprehensive performance of bismuth titanates high temperature piezoceramics；
(3) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and grind in mortar, obtain Powder；
(4) tabletting pre-burning: powder being placed in grinding tool and is pressed into material block in advance, will expect block pre-burning, and calcined temperature is 675 DEG C, is protected 4 hours warm time；
(5) secondary ball milling: by the material block after pre-burning in mortar, primary powder is obtained after being pulverized grinding, to what is obtained The dehydrated alcohol with primary powder equivalent is added in primary powder, continues ball milling 12 hours, is uniformly mixed powder and forms slurry；
(6) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and pulverize in mortar Material；
(7) poly-vinyl alcohol solution (PVA) that distilled water and concentration are 8% granulating and forming: is mixed into powder as adhesive In material, the quality of the distilled water of incorporation is the 2.5% of powder quality, and the quality of the adhesive of incorporation is the 5% of powder quality, It is uniformly mixed in mortar；Mixed powder is placed in grinding tool, green compact are pressed into；Green compact are milled to powder in mortar, By the sieve of 60 mesh and 120 mesh, the powder of 60 mesh and 120 mesh sieve middle layers is taken, it is suitable to have obtained granular size Powder；Powder is placed in grinding tool, is pressed into green compact under the pressure of 200MPa；
(8) dumping: green compact dumping was excluded the PVA in green compact, obtain porcelain billet temperature lower calcination 3 hours of 650 DEG C；
(9) it is sintered: porcelain billet is sintered, sintering temperature is 1050 DEG C, soaking time 4 hours, obtains potsherd；
(10) it applies electrode: potsherd cleaning, drying, screen printing is brushed into silver electrode, silver ink firing, silver ink firing temperature 500~600 DEG C, soaking time 1~2 hour；
(11) it polarizes: the potsherd for having plated silver electrode being placed in 120~160 DEG C of silicone oil, polarizing voltage 12kV/mm ~15kV/mm, polarization time are 20min~40min.
Bi to be prepared in embodiment 1 as shown in fig. 14Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction of x=0.005 ceramics Figure and the curve of dielectric constant with temperature variation；Fig. 7 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics Curie temperature variation diagram；Fig. 8 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12The room temperature piezoelectric modulus of ceramics becomes Change figure；Fig. 9 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics 500 DEG C when change in resistance figure.
As seen from Figure 1, Cu/W manufactured in the present embodiment codoping modified bismuth titanate lead-free piezoelectric ceramics and pure phase Bismuth titanates piezoelectric ceramics XRD spectrum it is almost the same.
Test result is as follows: d33=31pC/N, TCElectricalresistivityρ=2.82 × 10 at=679 DEG C, 500 DEG C5Ω·cm。
Embodiment 2
Preparation meets chemical composition Bi4Ti3-x(Cu1/2W1/2)xO12, the Cu/W of x=0.01 codoping modified bismuth titanates (Bi4Ti3O12) leadless piezoelectric ceramics, including the following steps:
(1) ingredient: with Bi2O3Powder, TiO2Powder, CuO powder and WO3Powder is raw material, by Bi, Ti, Cu in general formula and The stoichiometry of W carries out ingredient；
(2) ball millings: the dehydrated alcohol with mixture equivalent being added into said mixture, continues ball milling 12 hours, It is uniformly mixed powder and forms slurry, it is possible thereby to further improve the comprehensive performance of bismuth titanates high temperature piezoceramics；
(3) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and grind in mortar, obtain Powder；
(4) tabletting pre-burning: powder being placed in grinding tool and is pressed into material block in advance, will expect block pre-burning, and calcined temperature is 675 DEG C, is protected 4 hours warm time；
(5) secondary ball milling: by the material block after pre-burning in mortar, primary powder is obtained after being pulverized grinding, to what is obtained The dehydrated alcohol with primary powder equivalent is added in primary powder, continues ball milling 12 hours, is uniformly mixed powder and forms slurry；
(6) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and pulverize in mortar Material；
(7) poly-vinyl alcohol solution (PVA) that distilled water and concentration are 8% granulating and forming: is mixed into powder as adhesive In material, the quality of the distilled water of incorporation is the 2.5% of powder quality, and the quality of the adhesive of incorporation is the 5% of powder quality, It is uniformly mixed in mortar；Mixed powder is placed in grinding tool, green compact are pressed into；Green compact are milled to powder in mortar, By the sieve of 60 mesh and 120 mesh, the powder of 60 mesh and 120 mesh sieve middle layers is taken, it is suitable to have obtained granular size Powder；Powder is placed in grinding tool, is pressed into green compact under the pressure of 200MPa；
(8) dumping: green compact dumping was excluded the PVA in green compact, obtain porcelain billet temperature lower calcination 3 hours of 650 DEG C；
(9) it is sintered: porcelain billet is sintered, sintering temperature is 1050 DEG C, soaking time 4 hours, obtains potsherd；
(10) it applies electrode: potsherd cleaning, drying, screen printing is brushed into silver electrode, silver ink firing, silver ink firing temperature 500~600 DEG C, soaking time 1~2 hour；
(11) it polarizes: the potsherd for having plated silver electrode being placed in 120~160 DEG C of silicone oil, polarizing voltage 12kV/mm ~15kV/mm, polarization time are 20min~40min.
Bi to be prepared in embodiment 2 as shown in Figure 24Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction of x=0.01 ceramics Figure and the curve of dielectric constant with temperature variation；Fig. 7 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics Curie temperature variation diagram；Fig. 8 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12The room temperature piezoelectric modulus of ceramics becomes Change figure；Fig. 9 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics 500 DEG C when change in resistance figure.
As seen from Figure 2, Cu/W manufactured in the present embodiment codoping modified bismuth titanate lead-free piezoelectric ceramics and pure phase Bismuth titanates piezoelectric ceramics XRD spectrum it is almost the same.
Test result is as follows: d33=34pC/N, TCElectricalresistivityρ=1.52 × 10 at=680 DEG C, 500 DEG C6Ω·cm。
Embodiment 3
Preparation meets chemical composition Bi4Ti3-x(Cu1/2W1/2)xO12, the Cu/W of x=0.015 codoping modified bismuth titanates (Bi4Ti3O12) leadless piezoelectric ceramics, including the following steps:
(1) ingredient: with Bi2O3Powder, TiO2Powder, CuO powder and WO3Powder is raw material, by Bi, Ti, Cu in general formula and The stoichiometry of W carries out ingredient；
(2) ball millings: the dehydrated alcohol with mixture equivalent being added into said mixture, continues ball milling 12 hours, It is uniformly mixed powder and forms slurry, it is possible thereby to further improve the comprehensive performance of bismuth titanates high temperature piezoceramics；
(3) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and grind in mortar, obtain Powder；
(4) tabletting pre-burning: powder being placed in grinding tool and is pressed into material block in advance, will expect block pre-burning, and calcined temperature is 675 DEG C, is protected 4 hours warm time；
(5) secondary ball milling: by the material block after pre-burning in mortar, primary powder is obtained after being pulverized grinding, to what is obtained The dehydrated alcohol with primary powder equivalent is added in primary powder, continues ball milling 12 hours, is uniformly mixed powder and forms slurry；
(6) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and pulverize in mortar Material；
(7) poly-vinyl alcohol solution (PVA) that distilled water and concentration are 8% granulating and forming: is mixed into powder as adhesive In material, the quality of the distilled water of incorporation is the 2.5% of powder quality, and the quality of the adhesive of incorporation is the 5% of powder quality, It is uniformly mixed in mortar；Mixed powder is placed in grinding tool, green compact are pressed into；Green compact are milled to powder in mortar, By the sieve of 60 mesh and 120 mesh, the powder of 60 mesh and 120 mesh sieve middle layers is taken, it is suitable to have obtained granular size Powder；Powder is placed in grinding tool, is pressed into green compact under the pressure of 200MPa；
(8) dumping: green compact dumping was excluded the PVA in green compact, obtain porcelain billet temperature lower calcination 3 hours of 650 DEG C；
(9) it is sintered: porcelain billet is sintered, sintering temperature is 1050 DEG C, soaking time 4 hours, obtains potsherd；
(10) it applies electrode: potsherd cleaning, drying, screen printing is brushed into silver electrode, silver ink firing, silver ink firing temperature 500~600 DEG C, soaking time 1~2 hour；
(11) it polarizes: the potsherd for having plated silver electrode being placed in 120~160 DEG C of silicone oil, polarizing voltage 12kV/mm ~15kV/mm, polarization time are 20min~40min.
Bi to be prepared in embodiment 3 as shown in Figure 34Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction of x=0.015 ceramics Figure and the curve of dielectric constant with temperature variation；Fig. 7 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics Curie temperature variation diagram；Fig. 8 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12The room temperature piezoelectric modulus of ceramics becomes Change figure；Fig. 9 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics 500 DEG C when change in resistance figure.
As seen from Figure 3, Cu/W manufactured in the present embodiment codoping modified bismuth titanate lead-free piezoelectric ceramics and pure phase Bismuth titanates piezoelectric ceramics XRD spectrum it is almost the same.
Test result is as follows: d33=30pC/N, TCElectricalresistivityρ=7.73 × 10 at=675 DEG C, 500 DEG C6Ω·cm。
Embodiment 4
Preparation meets chemical composition Bi4Ti3-x(Cu1/2W1/2)xO12, the Cu/W of x=0.02 codoping modified bismuth titanates (Bi4Ti3O12) leadless piezoelectric ceramics, including the following steps:
(1) ingredient: with Bi2O3Powder, TiO2Powder, CuO powder and WO3Powder is raw material, by Bi, Ti, Cu in general formula and The stoichiometry of W carries out ingredient；
(2) ball millings: the dehydrated alcohol with mixture equivalent being added into said mixture, continues ball milling 12 hours, It is uniformly mixed powder and forms slurry, it is possible thereby to further improve the comprehensive performance of bismuth titanates high temperature piezoceramics；
(3) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and grind in mortar, obtain Powder；
(4) tabletting pre-burning: powder being placed in grinding tool and is pressed into material block in advance, will expect block pre-burning, and calcined temperature is 675 DEG C, is protected 4 hours warm time；
(5) secondary ball milling: by the material block after pre-burning in mortar, primary powder is obtained after being pulverized grinding, to what is obtained The dehydrated alcohol with primary powder equivalent is added in primary powder, continues ball milling 12 hours, is uniformly mixed powder and forms slurry；
(6) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and pulverize in mortar Material；
(7) poly-vinyl alcohol solution (PVA) that distilled water and concentration are 8% granulating and forming: is mixed into powder as adhesive In material, the quality of the distilled water of incorporation is the 2.5% of powder quality, and the quality of the adhesive of incorporation is the 5% of powder quality, It is uniformly mixed in mortar；Mixed powder is placed in grinding tool, green compact are pressed into；Green compact are milled to powder in mortar, By the sieve of 60 mesh and 120 mesh, the powder of 60 mesh and 120 mesh sieve middle layers is taken, it is suitable to have obtained granular size Powder；Powder is placed in grinding tool, is pressed into green compact under the pressure of 200MPa；
(8) dumping: green compact dumping was excluded the PVA in green compact, obtain porcelain billet temperature lower calcination 3 hours of 650 DEG C；
(9) it is sintered: porcelain billet is sintered, sintering temperature is 1050 DEG C, soaking time 4 hours, obtains potsherd；
(10) it applies electrode: potsherd cleaning, drying, screen printing is brushed into silver electrode, silver ink firing, silver ink firing temperature 500~600 DEG C, soaking time 1~2 hour；
(11) it polarizes: the potsherd for having plated silver electrode being placed in 120~160 DEG C of silicone oil, polarizing voltage 12kV/mm ~15kV/mm, polarization time are 20min~40min.
Bi to be prepared in embodiment 4 as shown in Figure 44Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction of x=0.02 ceramics Figure and the curve of dielectric constant with temperature variation；Fig. 7 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics Curie temperature variation diagram；Fig. 8 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12The room temperature piezoelectric modulus of ceramics becomes Change figure；Fig. 9 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics 500 DEG C when change in resistance figure.
As seen from Figure 4, Cu/W manufactured in the present embodiment codoping modified bismuth titanate lead-free piezoelectric ceramics and pure phase Bismuth titanates piezoelectric ceramics XRD spectrum it is almost the same.
Test result is as follows: d33=20pC/N, TCElectricalresistivityρ=3.31 × 10 at=675 DEG C, 500 DEG C6Ω·cm。
Embodiment 5
Preparation meets chemical composition Bi4Ti3-x(Cu1/2W1/2)xO12, the Cu/W of x=0.03 codoping modified bismuth titanates (Bi4Ti3O12) leadless piezoelectric ceramics, including the following steps:
(1) ingredient: with Bi2O3Powder, TiO2Powder, CuO powder and WO3Powder is raw material, by Bi, Ti, Cu in general formula and The stoichiometry of W carries out ingredient；
(2) ball millings: the dehydrated alcohol with mixture equivalent being added into said mixture, continues ball milling 12 hours, It is uniformly mixed powder and forms slurry, it is possible thereby to further improve the comprehensive performance of bismuth titanates high temperature piezoceramics；
(3) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and grind in mortar, obtain Powder；
(4) tabletting pre-burning: powder being placed in grinding tool and is pressed into material block in advance, will expect block pre-burning, and calcined temperature is 675 DEG C, is protected 4 hours warm time；
(5) secondary ball milling: by the material block after pre-burning in mortar, primary powder is obtained after being pulverized grinding, to what is obtained The dehydrated alcohol with primary powder equivalent is added in primary powder, continues ball milling 12 hours, is uniformly mixed powder and forms slurry；
(6) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and pulverize in mortar Material；
(7) poly-vinyl alcohol solution (PVA) that distilled water and concentration are 8% granulating and forming: is mixed into powder as adhesive In material, the quality of the distilled water of incorporation is the 2.5% of powder quality, and the quality of the adhesive of incorporation is the 5% of powder quality, It is uniformly mixed in mortar；Mixed powder is placed in grinding tool, green compact are pressed into；Green compact are milled to powder in mortar, By the sieve of 60 mesh and 120 mesh, the powder of 60 mesh and 120 mesh sieve middle layers is taken, it is suitable to have obtained granular size Powder；Powder is placed in grinding tool, is pressed into green compact under the pressure of 200MPa；
(8) dumping: green compact dumping was excluded the PVA in green compact, obtain porcelain billet temperature lower calcination 3 hours of 650 DEG C；
(9) it is sintered: porcelain billet is sintered, sintering temperature is 1050 DEG C, soaking time 4 hours, obtains potsherd；
(10) it applies electrode: potsherd cleaning, drying, screen printing is brushed into silver electrode, silver ink firing, silver ink firing temperature 500~600 DEG C, soaking time 1~2 hour；
(11) it polarizes: the potsherd for having plated silver electrode being placed in 120~160 DEG C of silicone oil, polarizing voltage 12kV/mm ~15kV/mm, polarization time are 20min~40min.
Bi to be prepared in embodiment 5 as shown in Figure 54Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction of x=0.03 ceramics Figure and the curve of dielectric constant with temperature variation；Fig. 7 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics Curie temperature variation diagram；Fig. 8 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12The room temperature piezoelectric modulus of ceramics becomes Change figure；Fig. 9 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics 500 DEG C when change in resistance figure.
As seen from Figure 5, Cu/W manufactured in the present embodiment codoping modified bismuth titanate lead-free piezoelectric ceramics and pure phase Bismuth titanates piezoelectric ceramics XRD spectrum it is almost the same.
Test result is as follows: d33=18pC/N, TCElectricalresistivityρ=3.16 × 10 at=671 DEG C, 500 DEG C6Ω·cm。
Embodiment 6
Preparation meets chemical composition Bi4Ti3-x(Cu1/2W1/2)xO12, the Cu/W of x=0.04 codoping modified bismuth titanates (Bi4Ti3O12) leadless piezoelectric ceramics, including the following steps:
(1) ingredient: with Bi2O3Powder, TiO2Powder, CuO powder and WO3Powder is raw material, by Bi, Ti, Cu in general formula and The stoichiometry of W carries out ingredient；
(2) ball millings: the dehydrated alcohol with mixture equivalent being added into said mixture, continues ball milling 12 hours, It is uniformly mixed powder and forms slurry, it is possible thereby to further improve the comprehensive performance of bismuth titanates high temperature piezoceramics；
(3) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and grind in mortar, obtain Powder；
(4) tabletting pre-burning: powder being placed in grinding tool and is pressed into material block in advance, will expect block pre-burning, and calcined temperature is 675 DEG C, is protected 4 hours warm time；
(5) secondary ball milling: by the material block after pre-burning in mortar, primary powder is obtained after being pulverized grinding, to what is obtained The dehydrated alcohol with primary powder equivalent is added in primary powder, continues ball milling 12 hours, is uniformly mixed powder and forms slurry；
(6) it dries: above-mentioned slurry being placed in constant temperature oven and is toasted, remove dehydrated alcohol, and pulverize in mortar Material；
(7) poly-vinyl alcohol solution (PVA) that distilled water and concentration are 8% granulating and forming: is mixed into powder as adhesive In material, the quality of the distilled water of incorporation is the 2.5% of powder quality, and the quality of the adhesive of incorporation is the 5% of powder quality, It is uniformly mixed in mortar；Mixed powder is placed in grinding tool, green compact are pressed into；Green compact are milled to powder in mortar, By the sieve of 60 mesh and 120 mesh, the powder of 60 mesh and 120 mesh sieve middle layers is taken, it is suitable to have obtained granular size Powder；Powder is placed in grinding tool, is pressed into green compact under the pressure of 200MPa；
(8) dumping: green compact dumping was excluded the PVA in green compact, obtain porcelain billet temperature lower calcination 3 hours of 650 DEG C；
(9) it is sintered: porcelain billet is sintered, sintering temperature is 1050 DEG C, soaking time 4 hours, obtains potsherd；
(10) it applies electrode: potsherd cleaning, drying, screen printing is brushed into silver electrode, silver ink firing, silver ink firing temperature 500~600 DEG C, soaking time 1~2 hour；
(11) it polarizes: the potsherd for having plated silver electrode being placed in 120~160 DEG C of silicone oil, polarizing voltage 12kV/mm ~15kV/mm, polarization time are 20min~40min.
Bi to be prepared in embodiment 6 as shown in Figure 64Ti3-x(Cu1/2W1/2)xO12, the XRD diffraction of x=0.04 ceramics Figure and the curve of dielectric constant with temperature variation；Fig. 7 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics Curie temperature variation diagram；Fig. 8 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12The room temperature piezoelectric modulus of ceramics becomes Change figure；Fig. 9 is different amounts of Cu/W doping Bi4Ti3-x(Cu1/2W1/2)xO12Ceramics 500 DEG C when change in resistance figure.
As seen from Figure 6, Cu/W manufactured in the present embodiment codoping modified bismuth titanate lead-free piezoelectric ceramics and pure phase Bismuth titanates piezoelectric ceramics XRD spectrum it is almost the same.
Test result is as follows: d33=18pC/N, TCElectricalresistivityρ=2.47 × 10 at=668 DEG C, 500 DEG C6Ω·cm。

Claims (6)

1. a kind of Ti Cu/W codope bismuth titanates high temperature piezoceramics, which is characterized in that the piezoceramic material leads to Formula is Bi4Ti3-x(Cu1/2W1/2)xO12, wherein 0 < x≤0.04.
2. Ti Cu/W codope bismuth titanates high temperature piezoceramics according to claim 1, which is characterized in that x= 0.005,0.01,0.015,0.02,0.03 or 0.04.
3. a kind of preparation method of Ti Cu/W codope bismuth titanates high temperature piezoceramics, which is characterized in that including as follows Step: ingredient, drying, tabletting pre-burning, secondary ball milling, drying, granulating and forming, dumping, sintering, applies electrode, pole at ball milling Change；Wherein,
Ingredient: with Bi2O3Powder, TiO2Powder, CuO powder and WO3Powder is raw material, by Formula B i4Ti3-x(Cu1/2W1/2)xO12 The stoichiometry of middle Bi, Ti, Cu and W carry out ingredient, wherein 0 < x≤0.04；
Ball milling: the dehydrated alcohol with mixture equivalent being added into said mixture, continues ball milling 12~24 hours, makes powder Body is uniformly mixed and forms slurry, it is possible thereby to further improve the comprehensive performance of bismuth titanates high temperature piezoceramics；
Drying: above-mentioned slurry being placed in constant temperature oven and is toasted, and is removed dehydrated alcohol, and grind in mortar, is obtained powder；
Tabletting pre-burning: powder being placed in grinding tool and is pressed into material block in advance, will expect block pre-burning, and calcined temperature is 675~750 DEG C, heat preservation Time 2~4 hours；
Secondary ball milling: by the material block after pre-burning in mortar, primary powder is obtained after being pulverized grinding, to obtained primary powder The dehydrated alcohol of middle addition and primary powder equivalent continues ball milling 12~24 hours, is uniformly mixed powder and forms slurry；
Drying: above-mentioned slurry being placed in constant temperature oven and is toasted, and removes dehydrated alcohol, and powder is ground into mortar；
Granulating and forming: the poly-vinyl alcohol solution (PVA) that distilled water and concentration are 8% is mixed in powder as adhesive, is mixed The quality of the distilled water entered is the 2.5% of powder quality, and the quality of the adhesive of incorporation is the 5% of powder quality, in mortar It is uniformly mixed；Mixed powder is placed in grinding tool, green compact are pressed into；Green compact are milled to powder in mortar, pass through 60 The sieve of mesh and 120 mesh takes the powder of 60 mesh and 120 mesh sieve middle layers, has obtained the suitable powder of granular size；It will Powder is placed in grinding tool, is pressed into green compact under the pressure of 200MPa；
Dumping: green compact dumping was excluded the PVA in green compact, obtains porcelain billet temperature lower calcination 3 hours of 650 DEG C；
Sintering: porcelain billet is sintered, and sintering temperature is 1000~1100 DEG C, soaking time 2~4 hours, obtains potsherd；
It applies electrode: potsherd cleaning, drying, screen printing is brushed into silver electrode, silver ink firing, 500~600 DEG C of silver ink firing temperature, when heat preservation Between 1~2 hour；
Polarization: the potsherd for having plated silver electrode being placed in 120~160 DEG C of silicone oil, and polarizing voltage is 12kV/mm~15kV/ Mm, polarization time are 20min~40min.
4. the preparation method of Ti Cu/W codope bismuth titanates high temperature piezoceramics according to claim 3, special Sign is, during a ball milling and secondary ball milling, the Ball-milling Time is 12 hours.
5. the preparation method of Ti Cu/W codope bismuth titanates high temperature piezoceramics according to claim 3, special Sign is, in the burn-in process, the calcined temperature is 675 DEG C, and the soaking time is 4 hours.
6. the preparation method of Ti Cu/W codope bismuth titanates high temperature piezoceramics according to claim 3, special Sign is, in the sintering process, the sintering temperature is 1050 DEG C, and the soaking time is 4 hours.
CN201910009551.7A 2019-01-04 2019-01-04 A kind of Ti Cu/W codope bismuth titanates high temperature piezoceramics and preparation method thereof Pending CN109467428A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910009551.7A CN109467428A (en) 2019-01-04 2019-01-04 A kind of Ti Cu/W codope bismuth titanates high temperature piezoceramics and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910009551.7A CN109467428A (en) 2019-01-04 2019-01-04 A kind of Ti Cu/W codope bismuth titanates high temperature piezoceramics and preparation method thereof

Publications (1)

Publication Number Publication Date
CN109467428A true CN109467428A (en) 2019-03-15

Family

ID=65677564

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910009551.7A Pending CN109467428A (en) 2019-01-04 2019-01-04 A kind of Ti Cu/W codope bismuth titanates high temperature piezoceramics and preparation method thereof

Country Status (1)

Country Link
CN (1) CN109467428A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109837442A (en) * 2019-03-28 2019-06-04 北京工业大学 The preparation method of the nanocrystalline tungsten copper based composites of metal element Ti/Cr and the original position hard phase WC codope
CN113603472A (en) * 2021-08-17 2021-11-05 杭州电子科技大学 Preparation method of NiCuZn ferrite based on LTCC technology

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB201012637D0 (en) * 2010-07-28 2010-09-15 Univ Leeds Ceramic
CN101913860A (en) * 2010-08-19 2010-12-15 西北工业大学 Bismuth titanate based piezoelectric ceramic with high curie temperature and preparation method thereof
CN102167585A (en) * 2011-01-18 2011-08-31 北京科技大学 Multielement-doped bismuth titanate group lead-free piezoceramic material and preparation method thereof
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB201012637D0 (en) * 2010-07-28 2010-09-15 Univ Leeds Ceramic
CN101913860A (en) * 2010-08-19 2010-12-15 西北工业大学 Bismuth titanate based piezoelectric ceramic with high curie temperature and preparation method thereof
CN102167585A (en) * 2011-01-18 2011-08-31 北京科技大学 Multielement-doped bismuth titanate group lead-free piezoceramic material and preparation method thereof
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

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
HONGCHU DU ET AL.: "Preparation, Microstructure, and Ferroelectric Properties of Bi3.25La0.75Ti3-xMxO12 (M=Mo, W, Nb, V) Ceramics", 《J.PHYS.CHEM.C》 *
YUWEIZHAO ET AL.: "Enhanced electromechanical properties and conduction behaviors of Aurivillius Bi4Ti2.95(B1/3Nb2/3)0.05O12 (B=Mg, Zn,Cu) ceramics", 《MATERIALS LETTERS》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109837442A (en) * 2019-03-28 2019-06-04 北京工业大学 The preparation method of the nanocrystalline tungsten copper based composites of metal element Ti/Cr and the original position hard phase WC codope
CN113603472A (en) * 2021-08-17 2021-11-05 杭州电子科技大学 Preparation method of NiCuZn ferrite based on LTCC technology
CN113603472B (en) * 2021-08-17 2023-02-28 杭州电子科技大学 Preparation method of NiCuZn ferrite based on LTCC technology

Similar Documents

Publication Publication Date Title
CN109704761A (en) A kind of Nb Cr/Mo codope bismuth niobate calcium high temperature piezoceramics and preparation method thereof
CN1116247C (en) Low-loss PZT ceramic compositions cofirable with silver at reduced sintering temp and process for producing same
CN109574656A (en) A kind of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material and preparation method thereof
CN106554202B (en) A kind of bismuth laminated bismuth-sodium titanate high temperature piezoceramics and preparation method thereof
CN110698195B (en) High-resistivity and high-piezoelectric-activity bismuth calcium titanate-based high-temperature piezoelectric ceramic and preparation method thereof
CN109678497A (en) A kind of Ti Cu/Sb codope bismuth titanates high temperature piezoceramics and preparation method thereof
CN107244898B (en) Barium strontium titanate doped barium zirconate titanate calcium-based piezoelectric ceramic material and preparation method thereof
CN105367053B (en) A kind of low-loss X9R type multilayer ceramic capacitor dielectric material and preparation method thereof
CN109626988B (en) Piezoelectric ceramic material with high piezoelectric response and high Curie temperature and preparation method thereof
CN102910902B (en) BNT-BT-BKT-based perovskite system multielement lead-free piezoelectric ceramic and production method thereof
JP2008537724A (en) High power piezoelectric ceramic composition
CN102167585B (en) Multielement-doped bismuth titanate group lead-free piezoceramic material and preparation method thereof
CN113387697A (en) Sodium bismuth titanate-based ceramic material with high ferroelectric stability, ultra-fast charge and discharge and high energy storage efficiency and preparation method thereof
CN103172374A (en) Piezoelectric ceramic and piezoelectric device
CN102531638A (en) Additive and application thereof for reducing sintering temperature of piezoceramic
CN109467428A (en) A kind of Ti Cu/W codope bismuth titanates high temperature piezoceramics and preparation method thereof
CN103373849A (en) Niobium oxide doped barium calcium zirconate titanate leadless piezoelectric ceramic powder material
CN113213918B (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
CN102336567B (en) Ternary system high-temperature piezoelectric ceramic of magnesium bismuth titanate, bismuth zinc-based perovskite and lead titanate and preparation method thereof
CN103693958A (en) Anti-ferroelectric ceramic material for energy storage capacitor as well as preparation method and application thereof
CN109437889A (en) A kind of preparation method of Ti Cu/Ta codope bismuth titanates high temperature piezoceramics
CN102320831A (en) Zinc-bismuth based perovskite-lead titanate-lead based relaxor ferroelectric ternary system piezoceramics and preparation method thereof
CN101913860B (en) Bismuth titanate based piezoelectric ceramic with high curie temperature and preparation method thereof
CN115385675B (en) Bismuth ferrite based lead-free ferroelectric ceramic material with high Curie temperature and energy storage characteristic and preparation method thereof
CN109485414A (en) A kind of Ti Cu/Mo codope bismuth titanates high temperature piezoceramics 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
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190315