CN101050120A - Method for preparing bismuth ferrite based multifunctioanl oxide ceramic material - Google Patents
Method for preparing bismuth ferrite based multifunctioanl oxide ceramic material Download PDFInfo
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- CN101050120A CN101050120A CN 200710099070 CN200710099070A CN101050120A CN 101050120 A CN101050120 A CN 101050120A CN 200710099070 CN200710099070 CN 200710099070 CN 200710099070 A CN200710099070 A CN 200710099070A CN 101050120 A CN101050120 A CN 101050120A
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Abstract
This invention relates to a method for preparing BiFeO3-based multifunctional oxide ceramic. The method comprises: (1) pre-pressing BLTFO8 powder into a disc, loading oxide protective powder (Al2O3, CeO2, ZrO2 or FeO) into a graphite mold, and pressing; (2) transferring the BLTFO8 disc onto the oxide protective powder layer in the mold; (3) continuing adding oxide protective powder into the mold to embed the BLTFO8 disc, and pressing; (4) transferring the mold into an SPS sintering furnace, heating to 600 deg.C within 3 min, then heating to the sintering temperature at a rate of 50 deg.C/min, keeping the temperature, and sintering. Since BiFeO3 has G-type antiferromagnetic structure, doping with rare earth element such as La or Tb, or metal element such as Ba or K can alter its antiferromagnetic structure, and the obtained BiFeO3-based multifunctional oxide ceramic has ferromagnetism at room temperature. The method can inhibit the valency change of the elements and reduce loss, and the BiFeO3-based multifunctional oxide ceramic has good ferroelectric and ferromagnetic properties at room temperature.
Description
Technical field
The invention belongs to material science, the preparation and the sintering method of particularly multi-functional oxidation thing stupalith are mainly concerned with ferrous acid bismuth (BiFeO
3) base novel ferroelectric-ferromagnetic ceramic material and embedding discharge plasma sintering (SPS) technology.
Background technology
Along with electronic information technology, the continuous development of particularly mixed unicircuit and surface mounting technology, the new function ceramic components receives publicity more and more, and its development trend is mainly reflected in microminiaturization, multifunction, integrated, the high reliability of device.The ferroelectric-ferromagnetic multifunctional material has very strong competitive power under this demand for development.Wherein, BiFeO
3The base pottery at room temperature promptly has ferroelectric and ferromagnetic ordering simultaneously, for development provides the huge applications possibility based on the novel information stores processor of ferroelectric-integrated effect of magnetic and magnetoelectricity device etc.
There are two kinds of methods to prepare BiFeO at present
3The base pottery.Solid reaction process prepares BiFeO
3Bi can appear in the process of original washing powder body
2Fe
4O
9Deng dephasign, can obtain the higher BiFeO of purity after using rare nitric acid to clean
3Powder, but pottery still can be separated out dephasign in the pressureless sintering process, simultaneously, Fe appraises at the current rate and the appearance in oxygen room reduces material resistance in the sintering process, and the ferroelectricity of material disappears.Adopt quick liquid phase sintering technology, with Bi
2O
3And Fe
2O
3The powder ball milling mixes, and compressing tablet is placed on to be rapidly heated in the rapid heat-treatment furnace and carries out sintering more than the fusing point, can prepare high-resistance single-phase BiFeO
3Pottery.But there is following shortcoming in this method: to Bi
2O
3And Fe
2O
3The granularity of two kinds of powders and mixing uniformity have very strict requirement, must use the oxide powder of submicron order, and mixing will enough evenly just can obtain single-phase BiFeO
3Pottery; Simultaneously,, heat up rapidly because sintering time is short, the operability difficulty, the result's is repeated bad; The very flexible of sintering process, strict to 860 ℃ sintering temperatures restriction, too high or mistake is low all can to produce dephasign; In addition, the defectives such as processing very easily cracks that heat up fast, lower the temperature, density is low, can not prepare the bulk pottery.
Summary of the invention
The purpose of this invention is to provide a kind of ceramic dense degree height, loss is low, the preparation method of the bismuth ferrite based multifunctioanl oxide ceramic material that specific inductivity is stable.
The preparation method of the bismuth ferrite based multifunctioanl oxide ceramic material that the present invention proposes, it is characterized in that: described method contains following each step:
(1) BLTFO8 powder preparing:
A. iron nitrate, lanthanum nitrate and citric acid are mixed according to stoichiometric ratio, be mixed with clear solution, heated and stirred forms thickness colloidal sol;
B. in above-mentioned thickness colloidal sol, mix and add ammoniacal liquor adjusting pH value;
C. the Bismuth trinitrate that slowly adds chemical dosage ratio then to avoid the sedimentary appearance of Vikaline, stirs and makes its thorough mixing;
D. mixture is placed baking oven, form xerogel 120 ℃ of insulations;
E. gel slowly is warmed up to 200 ℃, dying fire takes place, remove organism,, obtain the BLTFO8 powder in 860 ℃ of rapid thermal process, insulation from spreading decomposition reaction.
(2) BLTFO8 pottery preparation:
A. take by weighing the BLTFO8 powder, be pressed into disk in advance;
B. oxide compound protectiveness powder is put into graphite jig, compacting;
C. on the oxide compound protectiveness powder layer in the compressing tablet immigration mould, adjust to the central position;
D. continue in mould, to add oxide compound protectiveness powder, with the embedding of BLTFO8 disk, compacting;
E. then mould is moved in the SPS sintering oven, rose to 600 ℃ at 3 minutes with interior, the speed with 50 ℃/min rises to sintering temperature then, insulation, and sintering, sintering pressure are 50MPa.
F. take out sample after sintering is finished, the oxide compound protectiveness powder of outside is removed, promptly obtain the BLTFO8 pottery.
In above-mentioned BLTFO8 powder preparation method, citric acid and all metal ions mol ratio are 1.5: 1 in a step of described step (1).
In above-mentioned BLTFO8 ceramic preparation, it is characterized in that: oxide compound protectiveness powder is Al in the b step of described step (2)
2O
3, CeO
2, ZrO
2Or FeO.
The purpose of this invention is to provide a kind of BiFeO
3The sintering process that the base pottery is new.Discharge plasma sintering technique has very big competitive power with quick low temperature dense sintering in the preparation of special cermacis, but because the use of graphite jig, can cause strongly reducing atmosphere, cause the generation in appraising at the current rate of element and oxygen room more than the critical sintering temperature easily at certain, worsen the electrical property of sample, this also is the shortcoming that the SPS sintered ceramic oxide all need overcome.Most oxide ceramics can be removed the carbon that infiltrates sample by the thermal treatment in later stage, remedy the oxygen room.But, BiFeO
3Matrix ties up to the Fe that produces in the reducing atmosphere
3+To Fe
2+Appraise at the current rate and be difficult to improve by later stage thermal treatment.For avoiding the infiltration of carbon in sample, we are by introducing protectiveness powder (Al
2O
3, CeO
2, ZrO
2, the FeO oxide powder) carry out the embedding sintering, can enlarge SPS The Application of Technology scope, in some extraordinary oxide ceramics sintering, used.With BiFeO
3The based ceramic powder body places graphite jig to add the protectiveness powder and carries out embedding through pre-tablet forming, and sintering number minute in the SPS sintering oven can obtain fine and close BiFeO
3The base pottery.
Because BiFeO
3Have G-type anti-ferromagnetic structure, at room temperature can only present extremely weak ferromegnetism.Destroy its anti-ferromagnetic structure by rare earth elements such as doping La, Tb, Dy, Ho or metallic elements such as Ba, K, Ca, make BiFeO
3The base pottery has room-temperature ferromagnetic.Adopt the embedding discharge plasma sintering, control sintering parameter can suppress appraising at the current rate of element, reduces the wastage, and makes doping BiFeO
3The base pottery at room temperature has good ferroelectric and ferromagnetic property simultaneously.
Description of drawings
The XRD figure of BLTFO8 spectrum among Fig. 1 embodiment 1
The room temperature magnetic hysteresis loop of BLTFO8 among Fig. 2 embodiment 1
3 minutes agglomerating product section micro-structure diagrams of 690 ℃ of insulations among Fig. 3 embodiment 2
The frequency spectrum of specific inductivity of product (a) and loss (b) among Fig. 4 embodiment 2
Synoptic diagram in protectiveness embedding SPS sintering (b) graphite jig among traditional SPS sintering (a) and the embodiment 3 among Fig. 5 embodiment 2
Among Fig. 6 embodiment 3 micro-structure diagram of 10 minutes sintering BLTFO8 potteries of 750 ℃ of insulations a) section (b) polishing carry out thermal etching in 30 minutes for back 650 ℃
The frequency spectrum of specific inductivity of product (a) and loss (b) among Fig. 7 embodiment 3
The ferroelectric hysteresis loop of BLTFO differing temps sintered product among Fig. 8 embodiment 3
Embodiment
Introduce below and use Al among the present invention
2O
3Powder protectiveness embedding discharge plasma sintering Bi
0.91La
0.05Tb
0.04FeO
3(BLTFO8) Tao Ci embodiment.
Embodiment 1:
Iron nitrate, lanthanum nitrate and citric acid are mixed (citric acid and all metal ions mol ratio are 1.5: 1) according to certain stoichiometric ratio, be mixed with clear solution, heated and stirred a few hours, form thickness colloidal sol, mix then and add ammoniacal liquor and regulate pH to 1.The Bismuth trinitrate that slowly adds chemical dosage ratio subsequently is to avoid the sedimentary appearance of Vikaline.Stir and made its thorough mixing in 30 minutes, place baking oven, form xerogel 120 ℃ of insulations.Gel slowly is warmed up to 200 ℃, dying fire takes place from spreading decomposition reaction, removes organism, 860 ℃ of rapid thermal process, insulation 5 minutes, obtains the BLTFO8 powder.X-ray diffraction analysis (XRD) test result shows that thing is the single-phase powder of R3c structure mutually.Under the room temperature, under the 60kOe test magnetic field, saturation magnetization can reach 1.4emu/g, and residual magnetization can reach 0.2emu/g.As shown in Figure 1 and Figure 2.
Embodiment 2:
Take by weighing an amount of BLTFO8 powder, put into graphite jig (Ф 15mm), the 20MPa compacting; Then mould is moved in the SPS sintering oven, use traditional SPS method to carry out sintering.Rose to 600 ℃ at 3 minutes with interior, the speed with 50 ℃/min rises to sintering temperature then, is incubated several minutes sintered samples.Take out sample after sintering is finished, carry out 2 hours thermal treatment de-carbons at 650 ℃.The dielectric properties of pottery are very responsive to sintering temperature: when sintering below 690 ℃, and ceramic loss low (tan δ is below 10%), specific inductivity is stablized (about 120), and the ceramic dense degree is low, and grain-size is about 1 micron; When surpassing 690 ℃, ceramic loss significantly increases, and dielectric properties worsen.As Fig. 3, Fig. 4, shown in Figure 5.
Embodiment 3:
Take by weighing an amount of BLTFO8 powder, 20MPa is pressed into the disk of Ф 12 * 2mm in advance; With a small amount of Al
2O
3Powder is put into graphite jig (Ф 15mm), 20MPa compacting; The Al in the compressing tablet immigration mould
2O
3On the layer, adjust to the central position; Continue in mould, to add Al
2O
3Powder uses the 20MPa compacting with the embedding of BLTFO8 disk; Then mould is moved in the SPS sintering oven, rose to 600 ℃ at 3 minutes with interior, the speed with 50 ℃/min rises to sintering temperature then, is incubated several minutes sintered samples.Sintering pressure is 50MPa.After finishing, takes out sintering sample, with the Al of outside
2O
3Powder removes, and promptly obtains the BLTFO8 pottery.When sintering below 850 ℃, the dielectric properties of pottery are insensitive to temperature variation, ceramic dense degree height (＞99%), and loss low (tan δ＜10%), specific inductivity is stable (about 120) relatively, and saturated polarization is at 20 μ C/cm
2As Fig. 6, Fig. 7, shown in Figure 8.
Embodiment 4:
Take by weighing an amount of BLTFO8 powder, 20MPa is pressed into the disk of Ф 12 * 2mm in advance; Small amount of Fe O powder is put into graphite jig (Ф 15mm), 20MPa compacting; On the FeO layer in the compressing tablet immigration mould, adjust to the central position; Continue in mould, to add the FeO powder, use the 20MPa compacting the embedding of BLTFO8 disk; Then mould is moved in the SPS sintering oven, rose to 600 ℃ at 3 minutes with interior, the speed with 50 ℃/min rises to 800 ℃ then, is incubated 10 minutes sintered samples.Sintering pressure is 50MPa.Take out sample after sintering is finished, the FeO powder of outside is removed, promptly obtain the BLTFO8 pottery.The dielectric properties of pottery are insensitive to temperature variation, ceramic dense (density＞99.9%), and loss low (tan δ＜8%), specific inductivity is stable (about 120) relatively, and saturated polarization is at 21 μ C/cm
2
Embodiment 5:
Take by weighing an amount of BLTFO8 powder, 20MPa is pressed into the disk of Ф 12 * 2mm in advance; With a small amount of CeO
2Powder is put into graphite jig (Ф 15mm), 20MPa compacting; The CeO in the compressing tablet immigration mould
2On the layer, adjust to the central position; Continue in mould, to add CeO
2Powder uses the 20MPa compacting with the embedding of BLTFO8 disk; Then mould is moved in the SPS sintering oven, rose to 600 ℃ at 3 minutes with interior, the speed with 50 ℃/min rises to 900 ℃ of insulations 5 minutes, sintered sample then.Sintering pressure is 20MPa.After finishing, takes out sintering sample, with the CeO of outside
2Powder removes, and promptly obtains the BLTFO8 pottery.The dielectric properties of pottery are insensitive to temperature variation, ceramic dense (density＞99.9%), and loss low (tan δ＜8%), specific inductivity is stablized (about 120), and saturated polarization is at 20 μ C/cm
2
Embodiment 6:
Take by weighing an amount of BLTFO8 powder, 20MPa is pressed into the disk of Ф 12 * 2mm in advance; With a small amount of ZrO
2Powder is put into graphite jig (Ф 15mm), 20MPa compacting; The ZrO in the compressing tablet immigration mould
2On the layer, adjust to the central position; Continue in mould, to add ZrO
2Powder uses the 20MPa compacting with the embedding of BLTFO8 disk; Then mould is moved in the SPS sintering oven, rose to 600 ℃ at 3 minutes with interior, the speed with 50 ℃/min rises to 750 ℃ of insulations 8 minutes, sintered sample then.Sintering pressure is 20MPa.After finishing, takes out sintering sample, with the ZrO of outside
2Powder removes, and promptly obtains the BLTFO8 pottery.The dielectric properties of pottery are insensitive to temperature variation, ceramic dense (density 97%), and loss low (tan δ＜10%), specific inductivity is stablized (about 120), and saturated polarization is at 17 μ C/cm
2
Claims (3)
1, the preparation method of bismuth ferrite based multifunctioanl oxide ceramic material is characterized in that: described method contains following each step:
(1) BLTFO8 powder preparing:
A. iron nitrate, lanthanum nitrate and citric acid are mixed according to stoichiometric ratio, be mixed with clear solution, heated and stirred forms thickness colloidal sol;
B. in above-mentioned thickness colloidal sol, mix and add ammoniacal liquor adjusting pH value;
C. the Bismuth trinitrate that slowly adds chemical dosage ratio then to avoid the sedimentary appearance of Vikaline, stirs and makes its thorough mixing;
D. mixture is placed baking oven, form xerogel 120 ℃ of insulations;
E. gel slowly is warmed up to 200 ℃, dying fire takes place, remove organism,, obtain the BLTFO8 powder in 860 ℃ of rapid thermal process, insulation from spreading decomposition reaction.
(2) BLTFO8 pottery preparation:
A. take by weighing the BLTFO8 powder, be pressed into disk in advance;
B. oxide compound protectiveness powder is put into graphite jig, compacting;
C. on the oxide compound protectiveness powder layer in the compressing tablet immigration mould, adjust to the central position;
D. continue in mould, to add oxide compound protectiveness powder, with the embedding of BLTFO8 disk, compacting;
E. then mould is moved in the SPS sintering oven, rose to 600 ℃ at 3 minutes with interior, the speed with 50 ℃/min rises to sintering temperature then, insulation, and sintering, sintering pressure are 50MPa.
F. take out sample after sintering is finished, the oxide compound protectiveness powder of outside is removed, promptly obtain the BLTFO8 pottery.
2, preparation method according to claim 1 is characterized in that: citric acid and all metal ions mol ratio are 1.5: 1 in a step of described step (1).
3, preparation method according to claim 1 is characterized in that: oxide compound protectiveness powder is Al in the b step of described step (2)
2O
3, CeO
2, ZrO
2Or FeO.
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|---|---|---|---|
| CN 200710099070 CN101050120A (en) | 2007-05-11 | 2007-05-11 | Method for preparing bismuth ferrite based multifunctioanl oxide ceramic material |
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|---|---|---|---|
| CN 200710099070 CN101050120A (en) | 2007-05-11 | 2007-05-11 | Method for preparing bismuth ferrite based multifunctioanl oxide ceramic material |
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| US20090108706A1 (en) * | 2007-10-24 | 2009-04-30 | Fujifilm Corporation | Ferroelectric oxide, process for producing the same, piezoelectric body, and piezoelectric device |
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| CN102173460A (en) * | 2011-02-25 | 2011-09-07 | 中国科学院新疆理化技术研究所 | Method for preparing bismuth ferrite material by thermal decomposition reaction |
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| CN101250056B (en) * | 2008-03-18 | 2013-01-02 | 中国科学院上海硅酸盐研究所 | Method for low-temperature preparation of pure phase oxide material |
| CN101279841B (en) * | 2008-05-22 | 2012-07-04 | 中国科学院电工研究所 | Method for preparing multi-ferroic material under intense magnetic field |
| CN101367671B (en) * | 2008-09-12 | 2011-01-12 | 济南大学 | Leadless double-layer ferro-electricity compound film for high temperature piezoelectric device and method of manufacturing the same |
| CN101632935B (en) * | 2009-07-19 | 2012-01-04 | 桂林理工大学 | Compound oxide photocatalyst Bi4V(2-x)AxO(11-3x/2) and preparation method thereof |
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| CN102173460A (en) * | 2011-02-25 | 2011-09-07 | 中国科学院新疆理化技术研究所 | Method for preparing bismuth ferrite material by thermal decomposition reaction |
| CN102320666B (en) * | 2011-06-21 | 2013-04-03 | 南京大学 | Preparation method for substituting fluorine for oxygen in bismuth ferrite crystal lattices |
| CN102320666A (en) * | 2011-06-21 | 2012-01-18 | 南京大学 | Preparation method for substituting fluorine for oxygen in bismuth ferrite crystal lattices |
| CN102856261A (en) * | 2012-09-07 | 2013-01-02 | 北京航空航天大学 | Method for preparing metal, ferroelectric substance, insulator and semiconductor structure |
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| CN106278240A (en) * | 2016-08-12 | 2017-01-04 | 内蒙古大学 | A kind of BiFeO3ceramic target and preparation method thereof |
| CN107993831A (en) * | 2017-12-04 | 2018-05-04 | 台州学院 | It is trace doped to induce ferromagnetic method and the compound of preparation |
| CN110015893A (en) * | 2019-05-20 | 2019-07-16 | 哈尔滨理工大学 | A kind of composite mixed bismuth ferrite-barium titanate binary system Lead-free ferroelectric ceramics material, preparation method and applications |
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