CN107986770A - Doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics and preparation method thereof - Google Patents
Doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics and preparation method thereof Download PDFInfo
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- CN107986770A CN107986770A CN201711167681.0A CN201711167681A CN107986770A CN 107986770 A CN107986770 A CN 107986770A CN 201711167681 A CN201711167681 A CN 201711167681A CN 107986770 A CN107986770 A CN 107986770A
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- oxide
- piezoelectric ceramics
- lead titanate
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- 239000000919 ceramic Substances 0.000 title claims abstract description 86
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 37
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 39
- 150000001875 compounds Chemical class 0.000 claims abstract description 16
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 11
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 10
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 10
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 10
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 10
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 10
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 10
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 10
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 10
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 10
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims description 47
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 40
- -1 Q oxide Inorganic materials 0.000 claims description 28
- 239000002994 raw material Substances 0.000 claims description 25
- 239000012254 powdered material Substances 0.000 claims description 24
- 238000005245 sintering Methods 0.000 claims description 24
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 23
- 238000000227 grinding Methods 0.000 claims description 21
- 230000010287 polarization Effects 0.000 claims description 21
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 16
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 16
- 239000003979 granulating agent Substances 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- 239000011812 mixed powder Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 229920002545 silicone oil Polymers 0.000 claims description 5
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- UDRRLPGVCZOTQW-UHFFFAOYSA-N bismuth lead Chemical compound [Pb].[Bi] UDRRLPGVCZOTQW-UHFFFAOYSA-N 0.000 claims 1
- 150000002085 enols Chemical class 0.000 claims 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 3
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 239000011575 calcium Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 230000002269 spontaneous effect Effects 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000010671 solid-state reaction Methods 0.000 description 2
- 229910002902 BiFeO3 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical class ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229960002415 trichloroethylene Drugs 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a kind of doping vario-property bismuth ferrite lead titanate piezoelectric ceramics and preparation method thereof.The piezoelectric ceramics is with following represented by formula I：mMnO2‑(1‑x‑y)Bi(1‑a)GaFe(1‑b)QbO3‑xPbTiO3‑yBaTiO3(I) wherein, 0.10≤x≤0.30,0.05≤y≤0.20,0 ＜ a≤0.30,0 ＜ b≤0.10,0≤m≤0.26；Wherein, G is any one in divalent alkaline-earth metal element B a, Ca, Sr, or any one in rare-earth metals La, Ce, Nb, Gd；Wherein, any one in Q Ti, Co, Cr, Ni element；Wherein, m MnO2Shared compound Bi(1‑a)GaFe(1‑b)QbO3‑PbTiO3‑BaTiO3Mass percent.The piezoelectric ceramics has the characteristics that resistivity is high, leakage current is low, dielectric constant is high, piezoelectric constant is high.
Description
Technical field
The present invention relates to piezoelectric ceramic technology field, more particularly, to a kind of doping vario-property bismuth ferrite-lead titanates piezoelectricity
Ceramics and preparation method thereof.
Background technology
Mutual conversion of the piezoelectric ceramics due to that can realize mechanical energy and electric energy with forward and inverse piezoelectric effect, conduct
A kind of important functional material is widely used in piezo-electric resonator, piezoelectric buzzer, piezoelectric filter, piezoelectric transformer, pressure
The high-technology fields such as electric loudspeaker, piezoelectrics and piezo-electric motor.
Bismuth ferrite-lead titanates (BF-PT) solid solution is perovskite structure, is had and PZT (lead titanate piezoelectric ceramics) class
As quasi- homotype phase boundary, be a kind of lead tolerance low (lead tolerance is only 20%), the piezoceramic material of high-curie temperature.In high temperature
Piezoelectric ceramics field has broad application prospects.However, the coercive field of BF-PT based piezoelectric ceramic materials is larger, this its pole made
Change process becomes extremely difficult.
In addition, the dielectric loss of BF-PT based piezoelectric ceramic materials is high, mechanical quality factor is low, this causes its piezoelectric property
Reduce.
The content of the invention
It is an object of the present invention to provide a kind of doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics and preparation method thereof
New solution.
According to the first aspect of the invention, there is provided a kind of doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics.The piezoelectricity is made pottery
Porcelain is with following represented by formula I：
mMnO2-(1-x-y)Bi(1-a)GaFe(1-b)QbO3-xPbTiO3-yBaTiO3 (I)
Wherein, 0.10≤x≤0.30,0.05≤y≤0.20,0 ＜ a≤0.30,0 ＜ b≤0.10,0≤m≤0.26；
Wherein, G be divalent alkaline-earth metal element B a, Ca, Sr in any one, or rare-earth metals La, Ce,
Any one in Nb, Gd；
Wherein, any one in Q Ti, Co, Cr, Ni element；
Wherein, m MnO2Shared compound Bi(1-a)GaFe(1-b)QbO3-PbTiO3-BaTiO3Mass percent.
Alternatively, 0.19≤x≤0.21,0.10≤y≤0.15,0.02≤a≤0.20,0.01≤b≤0.08,0.10≤
m≤0.20；
Alternatively, the doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics is perovskite structure.
According to the second aspect of the invention, there is provided a kind of preparation side of doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics
Method.The preparation method comprises the following steps：
Dispensing：
With MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3For raw material,
Various raw materials are according to chemical formula
mMnO2-(1-x-y)Bi(1-a)GaFe(1-b)QbO3-xPbTiO3-yBaTiO3In a, b, x, y, m setting value carry out
Weigh dispensing,
Wherein, 0.10≤x≤0.30,0.05≤y≤0.20,0 ＜ a≤0.30,0 ＜ b≤0.10,0≤m≤0.26；
Wherein, G be divalent alkaline-earth metal element B a, Ca, Sr in any one, or rare-earth metals La, Ce,
Any one in Nb, Gd；
Wherein, any one in Q Ti, Co, Cr, Ni element；
Wherein, m MnO2Shared compound Bi(1-a)GaFe(1-b)QbO3-PbTiO3-BaTiO3Mass percent；
Prepare：
By Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3Mixture carry out
Pre-burning, to obtain the first preburning powdered material,
MnO is added into first preburning powdered material2, and prepare and form mixed powder,
Granulating agent is added into the mixed powder, and is prepared into the crude green body of setting shape,
The crude green body is subjected to dumping processing,
The crude green body after dumping is handled is sintered, to obtain ceramic component；
Polarization：
Ceramic component is polarized, to obtain doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics.
Alternatively, it is described by Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3's
Mixture carries out pre-burning, and to obtain the first preburning powdered material the step of includes：
To Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3Mixture in plus
Enter absolute ethyl alcohol, and carry out first time mix grinding；
Mixture after first time mix grinding is dried；
Mixture after drying is subjected to pre-burning, to obtain the first preburning powdered material.
Alternatively, calcined temperature is 700-800 DEG C, when burn-in time is 8-10 small.
Alternatively, the temperature of the dumping processing is 500-600 DEG C, when the time of dumping processing is 3-5 small.
Alternatively, the granulating agent is the aqueous solution of polyvinyl alcohol, and the mass concentration of the aqueous solution of the polyvinyl alcohol is
4%-12%.
Alternatively, sintering temperature is 950-1150 DEG C, when sintering time is 5-10 small.
Alternatively, in the polarisation steps, including：Top electrode is plated on the ceramic component, and is put into silicone oil and applies
Add the direct current of 8-12kV/mm, to polarize, the polarization time is 15-30 minutes.
According to the third aspect of the invention we, there is provided a kind of preparation side of doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics
Method.The preparation method comprises the following steps：
Dispensing：
With MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3For raw material,
Various raw materials are according to chemical formula
mMnO2-(1-x-y)Bi(1-a)GaFe(1-b)QbO3-xPbTiO3-yBaTiO3In a, b, x, y, m setting value carry out
Weigh dispensing,
Wherein, 0.10≤x≤0.30,0.05≤y≤0.20,0 ＜ a≤0.30,0 ＜ b≤0.10,0≤m≤0.26；
Wherein, G be divalent alkaline-earth metal element B a, Ca, Sr in any one, or rare-earth metals La, Ce,
Any one in Nb, Gd；
Wherein, any one in Q Ti, Co, Cr, Ni element；
Wherein, m MnO2Shared compound Bi(1-a)GaFe(1-b)QbO3-PbTiO3-BaTiO3Mass percent.
Prepare：
By MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3Mixture
Pre-burning is carried out, to obtain the second preburning powdered material,
Granulating agent is added into second preburning powdered material, and is prepared into the crude green body of setting shape,
The crude green body is subjected to dumping processing,
The crude green body after dumping is handled is sintered, to obtain ceramic component；
Polarization：
Ceramic component is polarized, to obtain doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics.
Alternatively, it is described by MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And
BaCO3Mixture carry out pre-burning, to obtain the second preburning powdered material the step of includes：
To MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3Mixture
Middle addition absolute ethyl alcohol, and carry out mix grinding；
Mixture after mix grinding is dried；
Mixture after drying is subjected to pre-burning, to obtain the second preburning powdered material.
Alternatively, calcined temperature is 800-850 DEG C, when burn-in time is 3-8 small.
Alternatively, the temperature of the dumping processing is 500-600 DEG C, when the time of dumping processing is 3-5 small.
Alternatively, the granulating agent is the aqueous solution of polyvinyl alcohol, and the mass concentration of the aqueous solution of the polyvinyl alcohol is
4%-12%.
Alternatively, sintering temperature is 950-1150 DEG C, when sintering time is 5-10 small.
Alternatively, in the polarisation steps, including：Top electrode is plated on the ceramic component, and is put into silicone oil and applies
Add the direct current of 8-12kV/mm, to polarize, the polarization time is 15-30 minutes.
According to one embodiment of the disclosure, which has resistivity height, leakage
The characteristics of electric current is low, dielectric constant is high, piezoelectric constant is high.
In addition, the doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics has the characteristics that insulating properties is high.
In addition, the insulating properties of the doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics in high temperature environments is high.
By referring to the drawings to the present invention exemplary embodiment detailed description, further feature of the invention and its
Advantage will be made apparent from.
Brief description of the drawings
It is combined in the description and the attached drawing of a part for constitution instruction shows the embodiment of the present invention, and even
It is used to explain the principle of the present invention together with its explanation.
Fig. 1 is the flow chart of preparation method according to an embodiment of the invention.
Embodiment
Carry out the various exemplary embodiments of detailed description of the present invention now with reference to attached drawing.It should be noted that：Unless in addition have
Body illustrates that the unlimited system of component and the positioned opposite of step, numerical expression and the numerical value otherwise illustrated in these embodiments is originally
The scope of invention.
The description only actually at least one exemplary embodiment is illustrative to be never used as to the present invention below
And its application or any restrictions that use.
It may be not discussed in detail for technology, method and apparatus known to person of ordinary skill in the relevant, but suitable
In the case of, the technology, method and apparatus should be considered as part for specification.
In shown here and discussion all examples, any occurrence should be construed as merely exemplary, without
It is as limitation.Therefore, other examples of exemplary embodiment can have different values.
It should be noted that：Similar label and letter represents similar terms in following attached drawing, therefore, once a certain Xiang Yi
It is defined, then it need not be further discussed in subsequent attached drawing in a attached drawing.
According to one embodiment of present invention, there is provided a kind of doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics.The piezoelectricity
Ceramics are with following represented by formula I：
mMnO2-(1-x-y)Bi(1-a)GaFe(1-b)QbO3-xPbTiO3-yBaTiO3 (I)
Wherein, 0.10≤x≤0.30,0.05≤y≤0.20,0 ＜ a≤0.30,0 ＜ b≤0.10,0≤m≤0.26；
Wherein, G be divalent alkaline-earth metal element B a, Ca, Sr in any one, or rare-earth metals La, Ce,
Any one in Nb, Gd；
Wherein, any one in Q Ti, Co, Cr, Ni element；
Wherein, m MnO2Shared compound Bi(1-a)GaFe(1-b)QbO3-PbTiO3-BaTiO3Mass percent.
In the preparation, MnO2Added as sintering aid in raw material so that doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics
Sintering temperature significantly reduces, and reduces the volatilization of alkali metal source.
It should be noted that the value range of m is 0≤m≤0.26, i.e. MnO2Shared compound Bi(1-a)GaFe(1-b)QbO3-
PbTiO3-BaTiO3Molar percentage be 0-0.26%.
Doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics provided by the invention has resistivity height, leakage current is low, dielectric is normal
The characteristics of number is high, piezoelectric constant is high.
In addition, the doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics has the characteristics that insulating properties is high.
In addition, the insulating properties of the doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics in high temperature environments is high.
Preferably, in Formula I parameters scope, wherein, 0.19≤x≤0.21,0.10≤y≤0.15,0.02
≤ a≤0.20,0.01≤b≤0.08,0.10≤m≤0.20.
In the value range, the piezoelectric property of doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics is more excellent.
Preferably, which is perovskite structure.The piezoelectric ceramics material of the structure
The piezoelectric effect of material is good.
According to another embodiment of the invention, there is provided a kind of system of doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics
Preparation Method.As shown in Figure 1, the preparation method comprises the following steps：
S1, dispensing：
With MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3For raw material,
Various raw materials are according to chemical formula
mMnO2-(1-x-y)Bi(1-a)GaFe(1-b)QbO3-xPbTiO3-yBaTiO3In a, b, x, y, m setting value carry out
Weigh dispensing,
Wherein, 0.10≤x≤0.30,0.05≤y≤0.20,0 ＜ a≤0.30,0 ＜ b≤0.10,0≤m≤0.26；
Wherein, G be divalent alkaline-earth metal element B a, Ca, Sr in any one, or rare-earth metals La, Ce,
Any one in Nb, Gd；
Wherein, any one in Q Ti, Co, Cr, Ni element；
Wherein, m MnO2Shared compound Bi(1-a)GaFe(1-b)QbO3-PbTiO3-BaTiO3Mass percent.
Specifically, above-mentioned various raw materials are powder.Weighing is carried out according to the proportionate relationship of each element in Formula I to match somebody with somebody
Material.The dosage that those skilled in the art can set various raw materials according to being actually needed.
S2, preparation：
S21, by Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3Mixture
Pre-burning is carried out, to obtain the first preburning powdered material.
In one example, in this step, including：
To Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3Mixture in plus
Enter absolute ethyl alcohol, and carry out first time mix grinding, the solid material in above-mentioned raw materials is added with powder.The addition of absolute ethyl alcohol
The viscosity of raw material can be increased, so that first time mix grinding is more abundant, obtained powder is more finely, evenly.First time mix grinding
Carried out using the method for ball milling.
Preferably, when the first time mix grinding time is 10-40 small.Further, when the time of first time mix grinding is 20 small.
In intergrinding process, powder becomes more finely, evenly.
Then, the mixture after first time mix grinding is dried, to exclude the organic matters such as absolute ethyl alcohol.
Finally, the mixture after drying is subjected to pre-burning, to obtain the first preburning powdered material.The purpose of pre-burning is：Make each
Fully, uniformly, the solid solution that generation constituent is fixed, forms principal crystalline phase to the solid state reaction of raw material；And exclude raw material
In carbon dioxide and moisture, reduce crude green body burns till contraction, deformation, in order to control the appearance and size of ceramic.
Preferably, calcined temperature is 700-800 DEG C, when burn-in time is 8-10 small.Under the conditions of the pre-burning, each raw material
Solid state reaction more fully, evenly, and can effectively exclude the carbon dioxide and moisture in raw material.
S22, add MnO into the first preburning powdered material2, and prepare and form mixed powder.For example, in this step, including：
To addition MnO2The first preburning powdered material in add absolute ethyl alcohol, and carry out second of mix grinding.Similarly, the addition energy of absolute ethyl alcohol
Enough increase the viscosity of the first preburning powdered material, so that second of mix grinding is more abundant, the first obtained preburning powdered material is finer, more equal
It is even.
Powder after second of mix grinding is dried, to obtain mixed powder.Absolute ethyl alcohol can be excluded by drying,
Absolute ethyl alcohol is avoided to adversely affect follow-up sintering.For example, the method that second of mix grinding also uses ball milling.Preferably,
When the time of second of mix grinding is 20 small.Through second of mix grinding, thinner, mixed powder evenly has been obtained.
In the preparation, MnO2Added as sintering aid in raw material so that doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics
Sintering temperature significantly reduces, and reduces the volatilization of alkali metal source.
S23, add granulating agent into mixed powder, and is prepared into the crude green body of setting shape.For example, using mould compacting
Method shapes, and the size of obtained crude green body is Ф 10*2mm.The shape of crude green body is prepared according to the structure of piezoelectric patches.
Preferably, granulating agent is the aqueous solution of polyvinyl alcohol.The mass concentration of the aqueous solution of polyvinyl alcohol is 4%-12%.
The granulating agent has the characteristics of viscosity is high, and dosage is few.Further, the mass concentration of the aqueous solution of polyvinyl alcohol is 8%.This is dense
The granulating agent of degree, can form complete, uniform particle.
S24, by crude green body carry out dumping processing.The purpose of dumping is that the producing high-moleculars such as the polyvinyl alcohol in removal crude green body close
Thing, adversely affects to avoid to sintering.The phosphorus content of high-molecular compound is more, and when oxygen is insufficient, burning produces reduction
The very strong carbon monoxide of property.Oxide in raw material can be reduced to metal or low oxide by carbon monoxide.Metal is low
Valency oxide influences the color of ceramics, into performances such as porcelain, electrodepositable and polarization.
In one example, pre- dumping is carried out using organic solvent first.The pre- optional organic solvent of dumping is three chloroethenes
One kind in alkene, carbon tetrachloride, chloroform, acetone.
Then, the crude green body after pre- dumping is subjected to dumping processing at high temperature, the organic matters such as polyvinyl alcohol is thoroughly arranged
Remove.The temperature of dumping processing is 500-600 DEG C, when the time of dumping processing is 3-5 small.Under the conditions of being somebody's turn to do polyvinyl alcohol can be made contour
Molecular compound excludes completely.
In another example, crude green body is directly carried out to dumping processing at high temperature, in this way, can also be excluded
The high-molecular compounds such as polyvinyl alcohol.
S25, dumping is handled after crude green body be sintered, to obtain ceramic component.Sintering can with air sintering furnace into
OK.Preferably, sintering temperature is 950-1150 DEG C, when sintering time is 5-10 small.Crude green body is sintered under this condition, finally
Form the ceramic component of perovskite structure.The ceramic component is represented with compound I.There are all directions in the crystal of ceramic component
Spontaneous polarization, from polarity is not externally macroscopically presented.The identical region in spontaneous polarization direction is known as electricdomain.
S3, polarization：
Ceramic component is polarized, to obtain doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics.
Being turned to by the electricdomain of polarized ceramics element, i.e. polarization forces the spontaneous polarization of electricdomain to align, from
And make ceramic component that polarity be presented.
Preferably, in this step, including：First, top electrode is plated on ceramic component, in order to polarize.
Then, ceramic component is put into the direct current for applying 8-12kV/mm in silicone oil, to polarize, the polarization time is
15-30 minutes.
By polarization, ceramic component becomes the piezoelectric ceramic devices with piezoelectric property.
In other examples, ceramic component directly polarizes under atmospheric environment, ceramic component is had pressure
Electrical property.
According to another aspect of the present invention, there is provided a kind of preparation of doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics
Method.As shown in Figure 1, the preparation method comprises the following steps：
SS1, dispensing：
With MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3For raw material,
Various raw materials are according to chemical formula
mMnO2-(1-x-y)Bi(1-a)GaFe(1-b)QbO3-xPbTiO3-yBaTiO3In a, b, x, y, m setting value carry out
Weigh dispensing,
Wherein, 0.10≤x≤0.30,0.05≤y≤0.20,0 ＜ a≤0.30,0 ＜ b≤0.10,0≤m≤0.26；
Wherein, G be divalent alkaline-earth metal element B a, Ca, Sr in any one, or rare-earth metals La, Ce,
Any one in Nb, Gd；
Wherein, any one in Q Ti, Co, Cr, Ni element；
Wherein, m MnO2Shared compound Bi(1-a)GaFe(1-b)QbO3-PbTiO3-BaTiO3Mass percent.
Specifically, above-mentioned various raw materials are powder.In the preparation, doping vario-property bismuth ferrite-lead titanates can be significantly reduced
The sintering temperature of piezoelectric ceramics.
The dosage that those skilled in the art can set various raw materials according to being actually needed.
SS2, preparation：
SS21, by MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3's
Mixture carries out pre-burning, to obtain the second preburning powdered material.
In the method, all raw materials mix and directly carry out pre-burning, to obtain the second preburning powdered material.
For example, to MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3's
Absolute ethyl alcohol is added in mixture, and carries out mix grinding.For example, when the mix grinding time is 20 small, so that mixture is finer, more equal
It is even.After mix grinding, mixture is dried first, to exclude absolute ethyl alcohol.Then, mixture is subjected to pre-burning.By pre-burning, most
The second preburning powdered material is obtained eventually.The purpose of pre-burning is as previously described.
Preferably, in this step, calcined temperature is 800-850 DEG C, when burn-in time is 3-8 small.
Similarly, in the preparation, MnO2Added as sintering aid in raw material so that doping vario-property bismuth ferrite-lead titanates pressure
The sintering temperature of electroceramics significantly reduces, and reduces the volatilization of alkali metal source.
SS22, add granulating agent into the second preburning powdered material, and is prepared into the crude green body of setting shape.
Preferably, granulating agent is the aqueous solution of polyvinyl alcohol, and the mass concentration of the aqueous solution of polyvinyl alcohol is 4%-12%.
The granulating agent of the concentration, can form complete, uniform particle.
For example, being shaped using the method for mould compacting, the size of obtained crude green body is Ф 10*2mm.
SS23, by crude green body carry out dumping processing.The purpose of dumping is as previously described.
In one example, pre- dumping is carried out using organic solvent first.Optionally, organic solvent for trichloro ethylene,
One kind in carbon tetrachloride, chloroform, acetone.
Then, the crude green body after pre- dumping is subjected to dumping processing at high temperature, the organic matters such as polyvinyl alcohol is thoroughly arranged
Remove.Preferably, the temperature of dumping processing is 500-600 DEG C, when the time of dumping processing is 3-5 small.The treatment conditions can obtain
Good dumping effect.
In another example, crude green body is directly carried out to dumping processing at high temperature, in this way, can also be excluded
The organic matters such as polyvinyl alcohol.
SS24, dumping is handled after crude green body be sintered, to obtain ceramic component.Sintering can with air sintering furnace into
OK.Preferably, sintering temperature is 950-1150 DEG C, when sintering time is 5-10 small.Under the sintering condition, calcium titanium can be obtained
The ceramic component of ore deposit structure.The ceramic component is represented with compound I.There are the spontaneous pole of all directions in the crystal of ceramic component
Change, from polarity is not externally macroscopically presented.The identical region of spontaneous polarization is known as electricdomain.
SS3, polarization：
Ceramic component is polarized, to obtain doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics.Pass through polarized ceramics member
The electricdomain of part turns to, i.e. polarization forces the spontaneous polarization of electricdomain to align, so that polarity is presented in ceramic component.
Preferably, in this step, including：First, top electrode is plated on ceramic component, in order to polarize.
Then, ceramic component is put into the direct current for applying 8-12kV/mm in silicone oil, to polarize, the polarization time is
15-30 minutes.
By polarization, ceramic component is known as the piezoelectric ceramic devices with piezoelectric property.
In other examples, ceramic component directly polarizes under atmospheric environment, ceramic component is had pressure
Electrical property.
In the preparation method that two embodiments of the present invention provide, using A, B codope modes.Wherein, G elements pair
The Bi ions of substitution A, can reduce the lattice defect caused by Bi element evaporations, lift the heat endurance of bismuth ferrite material；And Q
Element substitutes the Fe ions of B, can reduce Lacking oxygen defect, reduces Fe ion concentrations.It can be reduced by this doping way
The leakage current of piezoelectric ceramics, improves resistivity, obtains the ferroelectric hysteresis loop of saturation.
In addition, by introducing energy and BiFeO3The unlimited BaTiO being dissolved and dielectric constant and piezoelectric constant are higher3, can carry
The insulating properties of boosting electroceramics.This causes piezoelectric ceramics to still ensure that higher insulating properties at high temperature, improves piezoelectric ceramics
Application performance in high temperature environments.
In addition, dielectric loss is reduced by Mn doping, to improve the dielectric properties of bismuth ferrite material.
It is excellent that for example, modified bismuth ferrite-lead titanate piezoelectric ceramics provided by the invention has, resistivity is high, dielectric loss is small etc.
Different in nature energy, its resistivity is up to 1012Ω m, dielectric loss is less than 0.02, and Curie temperature is higher than 620 DEG C.
Above-mentioned preparation method reduces the coercive field of doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics, improves resistivity,
Dielectric loss is reduced, improves the piezoelectric property of piezoelectric ceramics.
Although some specific embodiments of the present invention are described in detail by example, the skill of this area
Art personnel it should be understood that example above merely to illustrating, the scope being not intended to be limiting of the invention.The skill of this area
Art personnel are it should be understood that without departing from the scope and spirit of the present invention can modify above example.This hair
Bright scope is defined by the following claims.
Claims (10)
- A kind of 1. doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics, with following represented by formula I：mMnO2-(1-x-y)Bi(1-a)GaFe(1-b)QbO3-xPbTiO3-yBaTiO3 (I)Wherein, 0.10≤x≤0.30,0.05≤y≤0.20,0 ＜ a≤0.30,0 ＜ b≤0.10,0≤m≤0.26；Wherein, G is any one in divalent alkaline-earth metal element B a, Ca, Sr, or rare-earth metals La, Ce, Nb, Gd In any one；Wherein, any one in Q Ti, Co, Cr, Ni element；Wherein, m MnO2Shared compound Bi(1-a)GaFe(1-b)QbO3-PbTiO3-BaTiO3Mass percent.
- 2. doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics according to claim 1, wherein, 0.19≤x≤0.21, 0.10≤y≤0.15,0.02≤a≤0.20,0.01≤b≤0.08,0.10≤m≤0.20.
- 3. doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics according to claim 1, wherein, the doping vario-property ferrous acid Bismuth-lead titanate piezoelectric ceramics is perovskite structure.
- 4. a kind of preparation method of doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics, wherein, comprise the following steps：Dispensing：With MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3For raw material, various originals Material is according to chemical formulamMnO2-(1-x-y)Bi(1-a)GaFe(1-b)QbO3-xPbTiO3-yBaTiO3In the setting value of a, b, x, y, m weighed Dispensing,Wherein, 0.10≤x≤0.30,0.05≤y≤0.20,0 ＜ a≤0.30,0 ＜ b≤0.10,0≤m≤0.26；Wherein, G is any one in divalent alkaline-earth metal element B a, Ca, Sr, or rare-earth metals La, Ce, Nb, Gd In any one；Wherein, any one in Q Ti, Co, Cr, Ni element；Wherein, m MnO2Shared compound Bi(1-a)GaFe(1-b)QbO3-PbTiO3-BaTiO3Mass percent；Prepare：By Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3Mixture carry out pre-burning, To obtain the first preburning powdered material,MnO is added into first preburning powdered material2, and prepare and form mixed powder,Granulating agent is added into the mixed powder, and is prepared into the crude green body of setting shape,The crude green body is subjected to dumping processing,The crude green body after dumping is handled is sintered, to obtain ceramic component；Polarization：Ceramic component is polarized, to obtain doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics.
- 5. preparation method according to claim 4, wherein, it is described by Bi2O3, G oxide or carbide, Fe2O3, Q Oxide, PbO, TiO2And BaCO3Mixture carry out pre-burning, to obtain the first preburning powdered material the step of includes：To Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3Mixture in add nothing Water-ethanol, and carry out first time mix grinding；Mixture after first time mix grinding is dried；Mixture after drying is subjected to pre-burning, to obtain the first preburning powdered material.
- 6. preparation method according to claim 5, wherein, calcined temperature is 700-800 DEG C, and burn-in time is small for 8-10 When.
- 7. preparation method according to claim 4, wherein, the granulating agent is the aqueous solution of polyvinyl alcohol, the poly- second The mass concentration of the aqueous solution of enol is 4%-12%.
- 8. preparation method according to claim 4, wherein, sintering temperature is 950-1150 DEG C, and sintering time is small for 5-10 When.
- 9. preparation method according to claim 4, wherein, in the polarisation steps, including：On the ceramic component Top electrode is plated, and is put into the direct current for applying 8-12kV/mm in silicone oil, to polarize, the polarization time is 15-30 minutes.
- 10. a kind of preparation method of doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics, wherein, comprise the following steps：Dispensing：With MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3For raw material, various originals Material is according to chemical formulamMnO2-(1-x-y)Bi(1-a)GaFe(1-b)QbO3-xPbTiO3-yBaTiO3In the setting value of a, b, x, y, m weighed Dispensing,Wherein, 0.10≤x≤0.30,0.05≤y≤0.20,0 ＜ a≤0.30,0 ＜ b≤0.10,0≤m≤0.26；Wherein, G is any one in divalent alkaline-earth metal element B a, Ca, Sr, or rare-earth metals La, Ce, Nb, Gd In any one；Wherein, any one in Q Ti, Co, Cr, Ni element；Wherein, m MnO2Shared compound Bi(1-a)GaFe(1-b)QbO3-PbTiO3-BaTiO3Mass percent；Prepare：By MnO2、Bi2O3, G oxide or carbide, Fe2O3, Q oxide, PbO, TiO2And BaCO3Mixture carry out Pre-burning, to obtain the second preburning powdered material,Granulating agent is added into second preburning powdered material, and is prepared into the crude green body of setting shape,The crude green body is subjected to dumping processing,The crude green body after dumping is handled is sintered, to obtain ceramic component；Polarization：Ceramic component is polarized, to obtain doping vario-property bismuth ferrite-lead titanate piezoelectric ceramics.
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| CN111320468A (en) * | 2020-03-03 | 2020-06-23 | 北京科技大学 | Preparation method of doped bismuth ferrite-barium titanate lead-free piezoelectric ceramic material |
| CN111620683A (en) * | 2020-05-18 | 2020-09-04 | 哈尔滨工业大学 | High-energy-storage-density ceramic block with core-shell structure and preparation method thereof |
| CN112537955A (en) * | 2020-12-18 | 2021-03-23 | 济南大学 | Doped modified bismuth scandate-lead titanate-bismuth ferrite ternary system piezoelectric ceramic and dipole transmitting transducer thereof |
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