CN109704760A - A kind of single-phase multiferroic ceramics and preparation method thereof with this structure non-stoichiometric of viral in Austria - Google Patents
A kind of single-phase multiferroic ceramics and preparation method thereof with this structure non-stoichiometric of viral in Austria Download PDFInfo
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- CN109704760A CN109704760A CN201910012670.8A CN201910012670A CN109704760A CN 109704760 A CN109704760 A CN 109704760A CN 201910012670 A CN201910012670 A CN 201910012670A CN 109704760 A CN109704760 A CN 109704760A
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Abstract
The present invention provides a kind of SrBi with this structure non-stoichiometric of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9Single-phase multiferroic ceramics.Present invention employs analytically pure SrCO3、Bi2O3、Nb2O5、Co2O3And Fe2O3It is uniform by ball milling mixing after preparation, 750 ~ 850 DEG C pre-burning 2-4 hour, sieving and molding finally be sintereds 3-5 hours at a temperature of 1050-1100 DEG C, have obtained the single-phase SrBi with this structure non-stoichiometric of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9Single-phase multiferroic ceramics.Ceramic material preparation process prepared by the present invention is simple, and raw material is cheap, and production cost is low.Strategy is adulterated by artificial adjustment, the Lacking oxygen in material is reduced, reduces the generation of leakage current in material, and the performance of material is allowed to obtain apparent improvement.
Description
Technical field
The invention belongs to single-phase multiferroic ceramic material fields, are related to a kind of single-phase with this structure of viral in Austria
SrBi2Nb1.8(Fe0.1Co0.1)xO9Multiferroic ceramics and preparation method thereof.
Background technique
Multi-ferroic material refer to include in the same phase of material the basic performance of two or more (containing two kinds) iron material
Material.Therefore, multi-ferroic material is a kind of novel and multifunctional material, before having wide application in spintronics and other field
Scape.Among this, in addition to needing that there is magnetoelectric effect below Curie temperature in view of multi-ferroic material in practical application, thus
The BiFeO of ferroelectric transition temperature and magnetic phase transition temperature all on room temperature3(bismuth ferrite) material becomes the multiferroic of most study
Ceramic material.However, BiFeO3The Lacking oxygen defect of multi-ferroic material causes material to exist, and electric leakage, coercive field is larger, low resistance
The problems such as rate.
The compound of this structure of viral is by two-dimensional perovskite and (Bi in Austria2O2)2+Layer is by certain regular symbiosis arrangement
It forms, its chemical general formula is (Bi2O2)2+(Am-1BmO3m+1)2-, many researchs at present are made by the element doping to the position B
Material obtains ferromagnetic property on ferroelectric basis not losing, but among the process of doping, due to B ions with mix
The valence state difference of heteroion will appear many Lacking oxygens in material, and the resistance and ferroelectric properties to material generate it is huge broken
It is bad.In SrBi of the invention2Nb2O9In material system, it may occur that following defect chemistry:
After co-doped by Fe and Co, material obtains excellent magnetic property, but leaks electrical conduction current to material electricity
The destruction of performance is also to increase the resistivity of material it will be apparent that so reduce the leakage electrical conduction current of material, be obtain it is a kind of new
The key point of the excellent multiferroic monophase materials of type.
Summary of the invention
The purpose of the present invention is to provide a kind of SrBi with this structure non-stoichiometric of viral in Austria2Nb1.8
(Fe0.1Co0.1)xO9Single-phase multiferroic ceramics and preparation method thereof make the Lacking oxygen in material by artificially adjusting doping strategy
It reduces instead the gap of iron ion, thus the less appearance of the leakage electrical conduction current of material, it will be apparent that enhance material
Resistance and ferroelectric properties.Following defect qualitative occurs for material internal:
Can from above reaction process it can be found that the point defect of material becomes the calking of iron ion from Lacking oxygen, from
And it is increased in the resistance for macroscopically making material.
To reach the above-mentioned performance being previously mentioned, the present invention adopts the following technical scheme:
A kind of single-phase SrBi with this structure non-stoichiometric of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9Multiferroic pottery
The preparation method of porcelain, specific steps include:
1) according to chemical formula SrBi2Nb1.8(Fe0.1Co0.1)xO9By analytically pure SrCO3、Bi2O3、Nb2O5、 Co2O3And
Fe2O3It is uniform by ball milling mixing after preparation, it then dries, be sieved, then through pre-burning, obtain blocks of solid；
2) after crushing blocks of solid, ball milling is carried out again, and product is sieved to obtain SrBi of uniform size2Nb1.8
(Fe0.1Co0.1)xO9Powder；
3) SrBi that will be obtained2Nb1.8(Fe0.1Co0.1)xO9Powder pours into compression moulding in mold, by the base of forming
Body is demoulded, and the intact green body of shape is obtained；
4) green body prepared carries out cold isostatic compaction；
5) obtained blank sintering is obtained into single-phase SrBi at porcelain2Nb1.8(Fe0.1Co0.1)xO9Multiferroic ceramics.
Mixed oxide in the step 1), step 2) mixes with zirconium ballstone and deionized water, ball milling, is formed after drying
Siccative, Ball-milling Time are 5~7 hours.
Pre-burning condition in the step 1) are as follows: heated up 750~850 DEG C with 5 DEG C/min, 2-4 hours are kept the temperature, later, with 5
DEG C/min is cooled to 500 DEG C, furnace cooling to room temperature.
In the step 4), cold isostatic compaction is the pressure for applying 200-250MPa in press, and the dwell time is
180-300s。
In the step 5), sintering condition is that 1050-1100 DEG C is raised to 5 DEG C/min, 3-5 hours is kept the temperature, later, with 5
DEG C/min is cooled to 500 DEG C, furnace cooling to room temperature.
A kind of single-phase SrBi with this structure non-stoichiometric of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9Multiferroic pottery
The method that porcelain is surface-treated, comprising the following steps: polishing, cleaning have the list of this structure non-stoichiometric of viral in Austria
Phase SrBi2Nb1.8(Fe0.1Co0.1)xO9Multiferroic ceramics uniformly coat silver electrode paste in the tow sides of ceramics, carry out hot place
Reason obtains the single-phase SrBi with this structure non-stoichiometric of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9Multiferroic ceramic electrical
Learn performance test sample.
It is a kind of to have it is difficult to understand in viral this structure non-stoichiometric single-phase SrBi2Nb1.8(Fe0.1Co0.1)xO9Multiferroic
The method of ceramic surface processing, the temperature of heat treatment are 800-850 DEG C, soaking time 15-20min.
Compared with prior art, the invention has the benefit that in the present invention, being adulterated by artificial controllable change
Strategy is transformed into the reaction of the defects of material for the process of (3) and (4) from (1) and (2), this transformation not only retains
The multiferroics of raw material itself, and the appearance of the caused Lacking oxygen of doping is avoided, to be obtained in terms of material resistance
Excellent promotion was obtained, the leakage current in material is reduced, the dielectric for the material that these results invent us, ferroelectricity
It can all be beneficial, and a good basis can be provided for subsequent magneto-electric coupled performance test.The sample of this experiment
In the preparation process of product, more advanced cold isostatic compaction technology is used, avoids waste and the binder of sample
It is added, saves the cost of production, accelerate the production cycle and avoid pollution of the binder to sample.In addition to this, by
It is that the transmitting of pressure, compared with the compacting of traditional individual event pressurization, isostatic cool pressing are carried out using liquid in cold isostatic compaction technology
Molding can allow sample to be under pressure from all directions, and pressure compares more greatly, and the green compact of preparation are more fine and close, be next
Excellent experimental result is walked to lay a good foundation.
Detailed description of the invention
Fig. 1 has the single-phase SrBi of this structure of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9The XRD spectrum of multiferroic ceramics,
SBCFN1:x=1, SBCFN2:x=5/3；
Fig. 2 has the single-phase SrBi of this structure of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9The scanned picture of multiferroic ceramics,
(a) x=1, (b) x=5/3；
Fig. 3 has the single-phase SrBi of this structure of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9The dielectric constant of multiferroic ceramics
Map, (a) x=1, (b) x=5/3 are varied with temperature at different frequencies；
Fig. 4: there is the single-phase SrBi of this structure of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9The polarization intensity of multiferroic ceramics
With the variation map of electric field, respectively sample is in different ferroelectric hysteresis loops off field.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and embodiments, but the present invention is not limited to following implementation
Example.
Embodiment one
A kind of single-phase SrBi with this structure non-stoichiometric of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9Multiferroic pottery
The preparation method of porcelain, wherein x indicates molar percentage, and x=1, specific steps include:
1) according to chemical formula SrBi2Nb1.8Fe0.1Co0.1O9By analytically pure SrCO3、Bi2O3、Nb2O5、Co2O3And Fe2O3
It is uniform by ball milling mixing after preparation, it then dries, be sieved, then through 800 DEG C of pre-burning 4h, obtain blocks of solid；
2) after crushing blocks of solid, ball milling is carried out again, and product is sieved to obtain of uniform size
SrBi2Nb1.8Fe0.1Co0.1O9Powder；
3) SrBi that will be obtained2Nb1.8Fe0.1Co0.1O9Powder pours into compression moulding in mold, by the green body of forming into
Row demoulding, obtains the intact green body of shape；
4) SrBi that will be obtained2Nb1.8Fe0.1Co0.1O9Powder is weighed with every part of quality 0.4g, is subsequently poured into mold
In the middle, the power for applying 600N demoulds the disk of forming, obtains the intact sample of shape；Disk is placed in gum cover
In the middle, the air of gum cover is discharged using vaccum-pumping equipment, sealant running-on is put into cold isostatic compaction, in the pressure of 200Mpa
Pressure maintaining 300s under power；
5) by obtained green body in 1070 DEG C of sintering 4h at porcelain, obtain single-phase SrBi2Nb1.8Fe0.1Co0.1O9Multiferroic ceramics；
6) polishing, cleaning step 5) in after once sintered good style, uniformly coat silver electrode in the tow sides of style
Slurry carries out heat treatment 15min at 850 DEG C, obtains SrBi2Nb1.8Fe0.1Co0.1O9Iron ceramic material sample.
Referring to Fig.1, SBCFN1 curve is sample XRD spectrum manufactured in the present embodiment in figure, is as can be seen from the figure synthesized
The SrBi of pure phase2Nb1.8Fe0.1Co0.1O9Ceramic material；
Referring to Fig. 2, figure (a) is the SEM picture that the present embodiment prepares sample, it can be seen that pure phase
SrBi2Nb1.8Fe0.1Co0.1O9Sheet-like morphology is presented in ceramic material crystal grain；
Referring to Fig. 3, figure (a) is Jie's temperature map that the present embodiment prepares sample；
Referring to Fig. 4, SBCFN1@75kV/cm is ferroelectric hysteresis loop of the sample of x=1 under the electric field of 75kV/cm in figure.
Embodiment two
A kind of single-phase SrBi with this structure non-stoichiometric of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9Multiferroic pottery
The preparation method of porcelain, wherein x indicates molar percentage, and x=5/3, specific steps include:
1) according to chemical formula SrBi2Nb1.8(Fe0.1Co0.1)5/3O9By analytically pure SrCO3、Bi2O3、Nb2O5、 Co2O3And
Fe2O3It is uniform by ball milling mixing after preparation, it then dries, be sieved, then through 800 DEG C of pre-burning 4h, obtain blocks of solid；
2) after crushing blocks of solid, ball milling is carried out again, and product is sieved to obtain SrBi of uniform size2Nb1.8
(Fe0.1Co0.1)5/3O9Powder；
3) SrBi that will be obtained2Nb1.8(Fe0.1Co0.1)5/3O9Powder pours into compression moulding in mold, by the base of forming
Body is demoulded, and the intact green body of shape is obtained；
4) SrBi that will be obtained2Nb1.8(Fe0.1Co0.1)5/3O9Powder is weighed with every part of quality 0.4g, is subsequently poured into
In mold, apply the power of 600N, the disk of forming is demoulded, obtains the intact sample of shape；Disk is placed in
In gum cover, the air of gum cover is discharged using vaccum-pumping equipment, sealant running-on is put into cold isostatic compaction, in 200Mpa
Pressure under pressure maintaining 300s；
5) by obtained green body in 1070 DEG C of sintering 4h at porcelain, obtain single-phase SrBi2Nb1.8(Fe0.1Co0.1)5/3O9Multiferroic pottery
Porcelain；
6) polishing, cleaning step 5) in after once sintered good style, uniformly coat silver electrode in the tow sides of style
Slurry carries out heat treatment 15min at 850 DEG C, obtains SrBi2Nb1.8(Fe0.1Co0.1)5/3O9Iron ceramic material sample.
Referring to Fig.1, SBCFN2 curve is sample XRD spectrum manufactured in the present embodiment in figure, is as can be seen from the figure synthesized
The SrBi of pure phase2Nb1.8(Fe0.1Co0.1)5/3O9Ceramic material；
Referring to Fig. 2, figure (b) is the SEM picture that the present embodiment prepares sample, it can be seen that the SrBi of pure phase2Nb1.8
(Fe0.1Co0.1)5/3O9Sheet-like morphology is presented in ceramic material crystal grain；
Referring to Fig. 3, figure (b) is Jie's temperature map that the present embodiment prepares sample；
Referring to Fig. 4, SBCFN2@75kV/cm is ferroelectric hysteresis loop of the sample of x=5/3 under the electric field of 75kV/cm in figure；
SBCFN2@138kV/cm is ferroelectric hysteresis loop of the sample of x=5/3 under the electric field of 138kV/cm.
Claims (9)
1. a kind of single-phase multiferroic ceramics with this structure non-stoichiometric of viral in Austria, which is characterized in that its chemical formula
For SrBi2Nb1.8(Fe0.1Co0.1)xO9, x=1 ~ 5/3.
2. a kind of preparation method of the single-phase multiferroic ceramics with viral in Austria this structure non-stoichiometric, feature exist
In using solid phase method, specific steps include:
1) according to chemical formula SrBi2Nb1.8(Fe0.1Co0.1)xO9By analytically pure SrCO3、Bi2O3、Nb2O5、Co2O3And Fe2O3Match
It is uniform by ball milling mixing after system, it then dries, be sieved, then through pre-burning, obtain blocks of solid；
2) after crushing blocks of solid, ball milling is carried out again, and product is sieved to obtain SrBi of uniform size2Nb1.8(Fe0.1Co0.1)xO9Powder；
3) SrBi that will be obtained2Nb1.8(Fe0.1Co0.1)xO9Powder pours into compression moulding in mold, by the green body of forming into
Row demoulding, obtains the intact green body of shape；
4) green body by step 3) preparation carries out cold isostatic compaction；
5) blank sintering for obtaining step 4) obtains having the single-phase SrBi of this structure of viral in Austria at porcelain2Nb1.8
(Fe0.1Co0.1)xO9Multiferroic ceramics.
3. a kind of single-phase multiferroic ceramics with viral in Austria this structure non-stoichiometric according to claim 2
Preparation method, which is characterized in that the mixed oxide in the step 1), step 2 mixes with zirconium ballstone and deionized water, ball
Siccative is formed after mill, drying, Ball-milling Time is 5 ~ 7 hours.
4. a kind of single-phase multiferroic ceramics with viral in Austria this structure non-stoichiometric according to claim 2
Preparation method, which is characterized in that pre-burning condition in the step 1) are as follows: heated up 750 ~ 850 DEG C with 5 DEG C/min, heat preservation 2-4 is small
When, later, 500 DEG C are cooled to 5 DEG C/min, furnace cooling to room temperature.
5. a kind of single-phase multiferroic ceramics with viral in Austria this structure non-stoichiometric according to claim 2
Preparation method, which is characterized in that in the step 4), cold isostatic compaction is the pressure for applying 200-250MPa in press,
Dwell time is 180-300s.
6. a kind of single-phase multiferroic ceramics with viral in Austria this structure non-stoichiometric according to claim 2
Preparation method, which is characterized in that in the step 5), sintering condition is that 1050-1100 DEG C is raised to 5 DEG C/min, and heat preservation 3-5 is small
When, later, 500 DEG C are cooled to 5 DEG C/min, furnace cooling to room temperature.
7. a kind of method that the single-phase multiferroic ceramics with this structure non-stoichiometric of viral in Austria are surface-treated,
Characterized by comprising the following steps: polishing, cleaning have it is difficult to understand in viral this structure non-stoichiometric it is single-phase
SrBi2Nb1.8(Fe0.1Co0.1)xO9Multiferroic ceramics uniformly coat silver electrode paste in the tow sides of ceramics, carry out hot place
Reason obtains the single-phase SrBi with this structure non-stoichiometric of viral in Austria2Nb1.8(Fe0.1Co0.1)xO9Multiferroic ceramic electrical
Learn performance test sample.
8. according to claim 7 a kind of to the ceramics of the single-phase multiferroic with this structure non-stoichiometric of viral in Austria
The method being surface-treated, it is characterised in that the temperature of heat treatment is 800-850 DEG C, soaking time 15-20min.
9. single-phase more iron with this structure non-stoichiometric of viral in Austria of any one of claim 8-9 the method preparation
Property ceramics.
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|---|---|---|---|---|
| CN1335284A (en) * | 2000-07-28 | 2002-02-13 | Tdk株式会社 | Piezoelectric ceramics |
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| CN103193469A (en) * | 2013-01-30 | 2013-07-10 | 中国科学技术大学 | Nine-layer-structure titanium iron bismuth cobalt oxide multiferroic ceramic material and preparation method thereof |
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2019
- 2019-01-07 CN CN201910012670.8A patent/CN109704760B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335284A (en) * | 2000-07-28 | 2002-02-13 | Tdk株式会社 | Piezoelectric ceramics |
| CN101681911A (en) * | 2006-11-08 | 2010-03-24 | 思美公司 | Correlated electron memory |
| CN103193469A (en) * | 2013-01-30 | 2013-07-10 | 中国科学技术大学 | Nine-layer-structure titanium iron bismuth cobalt oxide multiferroic ceramic material and preparation method thereof |
| CN109111222A (en) * | 2018-09-30 | 2019-01-01 | 陕西科技大学 | A kind of multiferroic ceramics and preparation method thereof with this structure of viral in Austria of Co doping |
Non-Patent Citations (1)
| Title |
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| MAO XY 等: ""Multiferroic Properties of Layer-Structured Bi5Fe0.5Co0.5Ti3O15 Ceramics"", 《APPLIED PHYSICS LETTERS》 * |
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