CN106145941A - A kind of rich zirconium lead zirconate titanate bismuth ferrite multiferroic ceramic material - Google Patents
A kind of rich zirconium lead zirconate titanate bismuth ferrite multiferroic ceramic material Download PDFInfo
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- CN106145941A CN106145941A CN201610645548.0A CN201610645548A CN106145941A CN 106145941 A CN106145941 A CN 106145941A CN 201610645548 A CN201610645548 A CN 201610645548A CN 106145941 A CN106145941 A CN 106145941A
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Abstract
The present invention relates to field of functional materials, specifically a kind of rich zirconium lead zirconate titanate bismuth ferrite multiferroic ceramic material, its chemical composition is: (1 x) Pb (Zr1‑yTiy)O3+ z wt%Nb2O5+xBiFeO3, wherein x=0.005～0.10, y=0.01～0.1, z=0.5～2.0.The present invention have selected rich zirconium Pb (Zr, the Ti) O that the lead zirconate titanate system of rich zirconium is modified by mixing niobium3Material and BiFeO3Material is combined, and regulation the Nomenclature Composition and Structure of Complexes is to improve material spontaneous polarization at room temperature and magnetic performance, it is achieved at room temperature ferroelectricity and ferromagnetic coexist and have preferable magnetoelectric effect.The cost of material that many ferroelectric substances of the present invention are used is relatively low, and preparation technology is simple and is prone to preserve and use, and can be applicable to the high-tech sectors such as energy conversion, sensitive detection and modern communications.
Description
Technical field
The present invention relates to technical field of function materials, specifically, be a kind of rich zirconium lead zirconate titanate-bismuth ferrite multiferroic pottery
Ceramic material.
Background technology
Multi-ferroic material refers to comprise two kinds and two or more ferrum physical property, such as ferroelectricity in the same phase of material
Coexist with ferromagnetism.In multi-ferroic material, some new effects can be produced between different ferrum performances, such as magnetoelectric effect
Deng.Just because of the effect that these are new so that multi-ferroic material has application prospect widely, can be widely used for sensing
Device, transducer, capacitor and storage device etc..Multi-ferroic material owing to being with a wide range of applications, recent years always by
Further investigation.BiFeO3It is that one shows ferroelectricity and the multi-ferroic material of magnetic (anti-ferromagnetism) the most simultaneously.Its
Ferroelectrie Curie temperature TC=830 DEG C, antiferromagnetic Ne&1&el temperature TN=370 DEG C, but owing to the electric leakage that bismuth ferrite is big makes its ferroelectricity
At room temperature being difficult to saturated polarization, the ferromagnetism of bismuth ferrite is the faintest simultaneously, it is impossible in reality application.Traditional 53/
47 type lead zirconate titanate (PZT) materials are then entirely without ferromagnetism.
Summary of the invention
It is an object of the invention to provide a kind of novel low cost room temperature multiferroic ceramic material, it is thus achieved that at room temperature ferromagnetic
Property and ferroelectricity coexist and there is magneto-electric coupled multi-ferroic material, be applied to sensor, energy harvester and information storage
Device etc..Described ceramic material is rich zirconium lead zirconate titanate (Pb (Zr, the Ti) O modified by niobium oxide3) ferroelectricity primitive and ferrous acid
Bismuth (BiFeO3) magnetic primitive formed, and is changed the ferroelectricity of specimen material by the proportioning changing lead zirconate titanate and bismuth ferrite
And ferromagnetism, it is thus achieved that the new function pottery that spontaneous polarization strength and magnetic performance can be regulated and controled by outfield.
A first aspect of the present invention, it is provided that a kind of rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material, its chemical composition
For: (1-x) Pb (Zr1-yTiy)O3+ z wt%Nb2O5+xBiFeO3, wherein x=0.005～0.10, y=0.01～0.1, z=
0.5～2.0.The spontaneous polarization of controlled material, magnetic performance and magnetoelectric effect is come by changing the Nomenclature Composition and Structure of Complexes.
In a preferred embodiment of the invention, described x=0.10, y=0.10, z=1.
In a preferred embodiment of the invention, described x=0.04, y=0.03, z=1.5.
In a preferred embodiment of the invention, described x=0.05, y=0.05, z=1.5.
The ceramics sample of the present invention at room temperature shows ferroelectricity and certain ferromagnetism.Different BiFeO3Content and not
Ferroelectricity ferromagnetism power with Zr/Ti sample is different, works as BiFeO3Content is when about 10%, and spontaneous polarization strength is maintained at
25μc/cm2Above, the remanent polarization of sample reaches 80memu/g.
Dielectric constant and the dielectric loss of the ceramic material of the present invention are adjustable, DIELECTRIC CONSTANT εrBetween 230～310, it is situated between
Electrical loss tan δ is between 1.5% to 2.5%.
The body of ceramic material of the present invention ties up to ferroelectricity and ferromagnetism in the range of room temperature and coexists and have the most magneto-electric coupled
Performance.
A second aspect of the present invention, it is provided that the preparation method of above-mentioned rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material,
Using conventional high temperature solid reaction process to prepare, raw material is Pb3O4, ZrO2, TiO2, Bi2O3, Fe2O3And Nb2O5Deng, according to described
Chemical composition carries out proportioning raw materials.
Preferably, the preparation method of described rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material comprises the following steps:
A) raw material adding deionized water ball milling to mix some hours, synthesize after drying briquetting, synthesis temperature is: 700
It is incubated 1 hour at DEG C, is warming up at 850 DEG C insulation two hours the most again；
B), after secondary ball milling, the powder of calcining is mixed and briquetting with the poly (vinyl alcohol) binder of concentration 6wt%, through 24
Hour homogenizing, then pelletize, be pressed into base substrate；
C) within 1-2 hour, porcelain is become at 1250 DEG C-1350 DEG C sintering again；
D) then cutting processing, then by silver, polarize, magnetize, to obtain final product.
Preferably, in described step b, the addition of the poly (vinyl alcohol) binder of concentration 6wt% is the 5-8wt% of powder.
Preferably, in described step d polarization electric field intensity be 3kv/mm, poling temperature is 100 DEG C, at room temperature with
5000 Oersted magnetic field intensity magnetize.
A third aspect of the present invention, it is provided that above-mentioned rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material is in preparation sensing
Application in device, transducer, capacitor, energy harvester or information storage unit.
The present invention have selected rich zirconium Pb (Zr, the Ti) O that the lead zirconate titanate system of rich zirconium is modified by mixing niobium3Material and BiFeO3
Material is combined, and regulation the Nomenclature Composition and Structure of Complexes is to improve material spontaneous polarization at room temperature and magnetic performance, it is achieved in room temperature
Lower ferroelectricity and ferromagnetic coexist and there is preferable magnetoelectric effect.
It is simple, with low cost, with lead zirconate titanate-bismuth ferrite many ferroelectricitys material that meaning of the present invention is to have invented technique
Material, regulation and control improve spontaneous polarization strength and the magnetic performance of this material.The raw material that many ferroelectric substances of the present invention are used becomes
This is relatively low, and preparation technology is simple and is prone to preserve and use, and can be applicable to energy conversion, sensitive detection and the contour skill of modern communications
Art field.
Detailed description of the invention
The detailed description of the invention provided the present invention below in conjunction with embodiment elaborates.
Embodiment 1
Lead zirconate titanate-bismuth ferrite ceramic material.Its chemical composition is:
(1-x)Pb(Zr1-yTiy)O3+ z% (weight) Nb2O5+xBiFeO3, wherein x=0.10, y=0.10, z=1
Concrete technical operation flow method is as follows:
1. weighing ball milling: according to (1-x) Pb (Zr1-yTiy)O3+ z% (weight) Nb2O5+xBiFeO3, wherein x=0.10, y
The formula stoichiometry that=0.10, z=1 are to be synthesized carries out proportioning, adds deionized water and puts into ball grinder ball milling, then to close
Some hours of suitable rotating speed ball milling.
2. drying tabletting: dried by the slurry after ball milling, the powder body after drying takes out after grinding and pours mould in a level pressure
Power lower sheeting.
3. pre-burning: tabletting is put into calcining synthesis in Muffle furnace.Synthesis temperature is to be incubated 1 hour at 700 DEG C, rises the most again
Temperature is incubated two hours to 850 DEG C.
4. secondary ball milling is dried: the tabletting after pre-burning is put in ball grinder after crushed, is situated between using deionized water as ball milling
Matter, carried out secondary ball milling, with some hours of suitable rotating speed ball milling.
5. homogenizing and granulating: the powder body after drying sieves, it is the poly-of 6wt% that the powder body after sieving adds 5-8wt% concentration
Vinyl alcohol.After mix homogeneously, powder body is placed in mould tabletting again, and at room temperature stands homogenizing 24 hours, carry out after homogenizing
Pelletize.
6. molding: the powder after pelletize is placed in mould tabletting under a certain pressure, it is ensured that the base substrate of molding has
Fixed mechanical strength and without layering and crackle.
7. plastic removal, sintering: the ceramic body after pressing molding is put in Muffle furnace, room temperature slowly heating up, (heat up speed
2 DEG C/min of rate) to 700 DEG C be incubated 1 hour, make the PVA of addition fully volatilize.Ceramic body after plastic removal puts into alumina crucible
The grog landfill sintering of middle ceramic powder.Pottery heating rate be 3 DEG C/min, sintering temperature between 1250～1300 DEG C it
Between, temperature retention time is 2 hours, Temperature fall afterwards, and furnace temperature is down to during room temperature take out pottery.
8. go up electrode and polarization: sinter into after the cleaved processing of ceramic material of porcelain by electrode, in 3kv/mm electric field intensity
Lower polarization, poling temperature is 100 DEG C. at room temperature magnetizes with 5000 Oersted magnetic field intensity.
The ferroelectric hysteresis loop of the lead zirconate titanate prepared by above-mentioned technique-bismuth ferrite ceramic material is that typical ferroelectric electric hysteresis returns
Line, saturated polarization is relatively big, is 33 μ C/cm2, the remanent magnetization of sample reaches 80memu/g, it is adaptable to collection of energy
Device and transducer mount etc..
Embodiment 2
Lead zirconate titanate-bismuth ferrite ceramic material.Its chemical composition is:
(1-x)Pb(Zr1-yTiy)O3+ z% (weight) Nb2O5+xBiFeO3, wherein x=0.04, y=0.03, z=1.5
Concrete technical operation flow method is as follows:
1. weighing ball milling: according to ((1-x) Pb (Zr1-yTiy)O3+ z% (weight) Nb2O5+xBiFeO3, wherein x=0.05, y
The formula stoichiometry that=0.03, z=1.5 are to be synthesized carries out proportioning, adds deionized water and puts into ball grinder ball milling, then with
Some hours of suitable rotating speed ball milling.
2. drying tabletting: dried by the slurry after ball milling, the powder body after drying takes out after grinding and pours mould in a level pressure
Power lower sheeting.
3. pre-burning: tabletting is put into calcining synthesis in Muffle furnace.Synthesis temperature is to be incubated 1 hour at 700 DEG C, rises the most again
Temperature is incubated two hours to 850 DEG C.
4. secondary ball milling is dried: the tabletting after pre-burning is put in ball grinder after crushed, is situated between using deionized water as ball milling
Matter, carried out secondary ball milling, with some hours of suitable rotating speed ball milling.
5. homogenizing and granulating: the powder body after drying sieves, it is the poly-of 6wt% that the powder body after sieving adds 5-8wt% concentration
Vinyl alcohol.After mix homogeneously, powder body is placed in mould tabletting again, and at room temperature stands homogenizing 24 hours, carry out after homogenizing
Pelletize.
6. molding: the powder after pelletize is placed in mould tabletting under a certain pressure, it is ensured that the base substrate of molding has
Fixed mechanical strength and without layering and crackle.
7. plastic removal, sintering: the ceramic body after pressing molding is put in Muffle furnace, room temperature slowly heating up, (heat up speed
2 DEG C/min of rate) to 700 DEG C be incubated 1 hour, make the PVA of addition fully volatilize.Ceramic body after plastic removal puts into alumina crucible
The grog landfill sintering of middle ceramic powder.Pottery heating rate be 3 DEG C/min, sintering temperature between 1280～1350 DEG C it
Between, temperature retention time is 2 hours, Temperature fall afterwards, and furnace temperature is down to during room temperature take out pottery.
8. go up electrode and polarization: sinter into after the cleaved processing of ceramic material of porcelain by electrode, in 3kv/mm electric field intensity
Lower polarization, poling temperature is 100 DEG C, at room temperature magnetizes with 5000 Oersted magnetic field intensity.
The lead zirconate titanate prepared by above-mentioned technique-bismuth ferrite ceramic material is under 2000 oersteds, and during 300kHz, dielectric is normal
Number relative change rate is 12%, it is adaptable to Sensitive Apparatus and phase shifting device etc..
Embodiment 3
Lead zirconate titanate-bismuth ferrite ceramic material.Its chemical composition is:
(1-x)Pb(Zr1-yTiy)O3+ z% (weight) Nb2O5+xBiFeO3, wherein x=0.05, y=0.05, z=1.5
Concrete technical operation flow method is as follows:
1. weighing ball milling: according to (1-x) Pb (Zr1-yTiy+ 1wt%Nb2O5)O3+xBiFeO3, wherein x=0.03, y=
0.05, z=1.5 formula stoichiometry to be synthesized carries out proportioning, adds deionized water and puts into ball grinder ball milling, then with suitable
When some hours of rotating speed ball milling.
2. drying tabletting: dried by the slurry after ball milling, the powder body after drying takes out after grinding and pours mould in a level pressure
Power lower sheeting.
3. pre-burning: tabletting is put into calcining synthesis in Muffle furnace.Synthesis temperature is to be incubated 1 hour at 700 DEG C, rises the most again
Temperature is incubated two hours to 850 DEG C.
4. secondary ball milling is dried: the tabletting after pre-burning is put in ball grinder after crushed, is situated between using deionized water as ball milling
Matter, carried out secondary ball milling, with some hours of suitable rotating speed ball milling.
5. homogenizing and granulating: the powder body after drying sieves, it is the poly-of 6wt% that the powder body after sieving adds 5-8wt% concentration
Vinyl alcohol.After mix homogeneously, powder body is placed in mould tabletting again, and at room temperature stands homogenizing 24 hours, carry out after homogenizing
Pelletize.
6. molding: the powder after pelletize is placed in mould tabletting under a certain pressure, it is ensured that the base substrate of molding has
Fixed mechanical strength and without layering and crackle.
7. plastic removal, sintering: the ceramic body after pressing molding is put in Muffle furnace, room temperature slowly heating up, (heat up speed
2 DEG C/min of rate) to 700 DEG C be incubated 1 hour, make the PVA of addition fully volatilize.Ceramic body after plastic removal puts into alumina crucible
The grog landfill sintering of middle ceramic powder.Pottery heating rate be 3 DEG C/min, sintering temperature between 1280～1320 DEG C it
Between, temperature retention time is 2 hours, Temperature fall afterwards, and furnace temperature is down to during room temperature take out pottery.
8. go up electrode and polarization: sinter into after the cleaved processing of ceramic material of porcelain by electrode, in 3kv/mm electric field intensity
Lower polarization, poling temperature is 100 DEG C, at room temperature magnetizes with 5000 Oersted magnetic field intensity.
The lead zirconate titanate prepared by above-mentioned technique-bismuth ferrite ceramic material, under 5000 Oersted magnetic field intensity, when additional
Electric field is when+2000v/mm is backwards to-2000v/mm, and the relative change rate of magnetic induction can reach about 15%, can apply
In information storage elements and phase modulator etc..
Below preferred embodiment to the invention is illustrated, but the invention is not limited to described
Embodiment, those of ordinary skill in the art it may also be made that all equivalents on the premise of the invention spirit
Modification or replacement, modification or the replacement of these equivalents are all contained in the application claim limited range.
Claims (9)
1. rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material, it is characterised in that its chemical composition is: (1-x) Pb
(Zr1-yTiy)O3+ z wt%Nb2O5+xBiFeO3, wherein x=0.005～0.10, y=0.01～0.1, z=0.5～2.0.
Rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material the most according to claim 1, it is characterised in that described x
=0.10, y=0.10, z=1.
Rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material the most according to claim 1, it is characterised in that described x
=0.04, y=0.03, z=1.5.
Rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material the most according to claim 1, it is characterised in that described x
=0.05, y=0.05, z=1.5.
5. according to the preparation method of the arbitrary described rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material of claim 1-4, its
Being characterised by, using conventional high temperature solid reaction process to prepare, raw material is Pb3O4, ZrO2, TiO2, Bi2O3, Fe2O3And Nb2O5。
The preparation method of rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material the most according to claim 5, its feature exists
In, comprise the following steps:
A) raw material adding deionized water ball milling to mix some hours, synthesize after drying briquetting, synthesis temperature is: at 700 DEG C
It is incubated 1 hour, is warming up at 850 DEG C insulation two hours the most again；
B), after secondary ball milling, the powder of calcining was mixed and briquetting with the poly (vinyl alcohol) binder of concentration 6wt%, through 24 hours
Homogenizing, then pelletize, be pressed into base substrate；
C) within 1-2 hour, porcelain is become at 1250 DEG C-1350 DEG C sintering again；
D) then cutting processing, then by silver, polarize, magnetize, to obtain final product.
The preparation method of rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material the most according to claim 6, its feature exists
In, in described step b, the addition of the poly (vinyl alcohol) binder of concentration 6wt% is the 5-8wt% of powder.
The preparation method of rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material the most according to claim 6, its feature exists
In, in described step d, the electric field intensity of polarization is 3kv/mm, and poling temperature is 100 DEG C, at room temperature with 5000 oersted magnetic
Field intensity magnetizes.
9. according to the arbitrary described rich zirconium lead zirconate titanate-bismuth ferrite multiferroic ceramic material of claim 1-4 prepare sensor,
Application in transducer, capacitor, energy harvester or information storage unit.
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| CN109293353A (en) * | 2018-09-03 | 2019-02-01 | 中国科学院上海硅酸盐研究所 | A kind of unleaded BiFeO of high energy storage density and high energy storage efficiency3Base ferroelectric ceramic material and preparation method thereof |
| CN109293353B (en) * | 2018-09-03 | 2021-05-25 | 中国科学院上海硅酸盐研究所 | Lead-free BiFeO with high energy storage density and high energy storage efficiency3Ferroelectric ceramic material and its preparation method |
| CN111348913A (en) * | 2020-03-29 | 2020-06-30 | 贵州振华红云电子有限公司 | High bandwidth piezoelectric ceramic and preparation method thereof |
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