CN101607818A - Has laminate structure ferrotianium cobalt acid bismuth stupalith of multi-ferrum property and preparation method thereof - Google Patents
Has laminate structure ferrotianium cobalt acid bismuth stupalith of multi-ferrum property and preparation method thereof Download PDFInfo
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- CN101607818A CN101607818A CNA2009101822591A CN200910182259A CN101607818A CN 101607818 A CN101607818 A CN 101607818A CN A2009101822591 A CNA2009101822591 A CN A2009101822591A CN 200910182259 A CN200910182259 A CN 200910182259A CN 101607818 A CN101607818 A CN 101607818A
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Abstract
Have laminate structure ferrotianium cobalt acid bismuth stupalith of multi-ferrum property and preparation method thereof, belong to the oxide ceramic material preparing technical field, Bi
4Ti
3O
12And BiCoO
3Implant BiFeO
3The middle Bi that forms
5Fe
0.5Co
0.5Ti
3O
15(BFCT).This technology advantages of simple has and existing liquid process favorable compatibility, and the specimen preparation temperature can cut down the consumption of energy greatly well below the preparation temperature of current technology, is convenient to industrialization production.In BFCT, because the octahedra arrangement of Fe-O and Co-O is comparatively orderly, thereby the part obtains the coupling between the Fe-O-Co, makes the magnetic height of sample.
Description
Technical field
The invention belongs to the oxide ceramic material preparing technical field, have the preparation technology of ferroelectric, ferromagnetic ferrotianium cobalt acid bismuth pottery when particularly having laminated perovskite structure.
Background technology
The magnetoelectricity multi-iron material is meant in certain warm area, shows ferroelectric preface and ferromagnetic/antiferromagnetic preface simultaneously, and has certain coupled material each other.Recently, this material is attracted attention day by day, on the one hand because it not only can be used in the research and development of ferroelectric and magnetic apparatus, it can utilize coupling between the magnetoelectricity what is more important, for the design and the application of equipment provides additional one degree of freedom, show very tempting application prospect thereby drive on ferro-resonance device and the magnetic tuning piezoelectric transducer at emerging spintronics, polymorphic information storage, electricity.Up to the present, in the multi-iron material of having found, the BiFeO3 with simple uhligite ABO3 type structure is a kind of unleaded environmentally friendly material, has ferroelectric Curie temperature and antiferromagnetic Neel temperature far above room temperature, thereby receives much concern.Up-to-date research shows that also the photochemical catalysis performance of BFO also has potential using value.However, the BFO material, no matter pottery and film morphology, all have some that shortcoming to be overcome is arranged, big as dielectric loss, leakage current is higher, ferroelectric residual polarization is less, coercive field is than big and its magnetic spin structure heterogeneous etc., in addition, the preparation of pure phase BFO material also has certain degree of difficulty, and these difficulties have hindered it and moved towards practical paces.In order to solve these difficulties, everybody has taked multiple means, as on preparation technology, proposed quick lqiuid phase sintering method and can obtain fine and close body material, in addition, ion doping and other ferroelectric material group structure sosoloid, also can improve the ferroelectric residual polarization of material, performances such as residual magnetization, its modification theory roughly be attributable to spacer by rhombus in opposite directions quadrature change mutually, thereby inspire ferroelectric residual polarization, and the volution spin preface of breaking BFO discharges ferromegnetism etc.Consider the about 62nm of spin spiralization cycle of BFO, nano level BFO also has ferromegnetism performance preferably.
Ferrotianium acid bismuth (Bi
5FeTi
3O
15, BFTO) being bismuth-containing shape uhligite magnetodielectric material layer by layer, its structure is along per 2 bismuth oxygen the layer ((Bi of c direction
2O
2)
2+) between clip the octahedra and octahedra composition of 1 iron oxygen (Fe-O) of 3 titanyls (Ti-O); BFTO also can regard as by 1 three layers of ferroelectric material Bi
4Ti
3O
12(BTO) with 1 how ferroelectric BiFeO of uhligite
3(BFO) combine, its many iron property derives from ferroelectric cell (BTO) and many iron unit (BFO) respectively.BFTO can effectively utilize the insulating effect of bismuth oxygen layer to suppress magnet unit because the leakage current that oxygen room and Fe multivalence attitude cause.Bibliographical information: the magnetic property of BFTO sample still shows as antiferromagnetism, its Neel temperature (T
N) near the 80K, ferroelectric-para-electric transformation temperature is near 1000K.
Summary of the invention
The objective of the invention is to provide a kind of novel lamellar to have ferroelectric, ferromagnetic many iron of magnetoelectricity stupalith simultaneously.
Stupalith of the present invention is a ferrotianium cobalt acid bismuth (BFCT), and its molecular structural formula is: Bi
5Fe
0.5Co
0.5Ti
3O
15
Because it is antiferromagnetic that the magnetic property of BFTO shows as localization,, but still fail to discharge magnetic property by breaking antiferromagnetic spiral preface although illustrate that the octahedra unitary arrangement of Fe-O is unordered among the BFTO.So need to select other scheme, improve magnetic property as being coupled by the change magnetic ion.If half the Fe ion among the BFTO is substituted with the Co ion, form new ferrotianium cobalt acid bismuth (Bi
5Fe
0.5Co
0.5Ti
3O
15, BFCT) material then can be realized the coupling between Fe, the Co ion, this being coupled with may show as ferromegnetism.Bi at ferrotianium cobalt acid bismuth
5Fe
0.5Co
0.5Ti
3O
15(BFCT) in, because the octahedra arrangement of Fe-O and Co-O is comparatively orderly, thereby the part obtains the coupling between the Fe-O-Co, makes the magnetic height of sample.
Another purpose of the present invention provides the preparation method of the stupalith of the ferrotianium cobalt acid bismuth with above-mentioned molecular structural formula.
This preparation technology is: prepare Bi earlier
4Ti
3O
12(BTO) powder is again with Bi
4Ti
3O
12(BTO) and BiCoO
3(BCO) implant BiFeO
3(BFO) form Bi in
5Fe
0.5Co
0.5Ti
3O
15(BFCT).
This technology advantages of simple has and existing liquid process favorable compatibility, and the specimen preparation temperature can cut down the consumption of energy greatly well below the preparation temperature of current technology, is convenient to industrialization production.
The concrete technical scheme of the present invention was divided into for two steps, the preparation of (1) BTO powder; (2) preparation of BFCT ceramics sample.
(1) Bi
4Ti
3O
12(BTO) preparation of powder: adopt traditional solid-phase sintering process, with analytical pure bismuth oxide (Bi
2O
3) and spectroscopically pure titanium oxide (TiO
2) be raw material, take by weighing raw material by stoicheiometry, carry out repeatedly synthetic at 760～800 ℃.
(2) Bi
5Fe
0.5Co
0.5Ti
3O
15(BFCT) preparation of ceramics sample: add analytical pure bismuth oxide (Bi by stoicheiometry with the BTO powder that has made
2O
3), analytical pure ferric oxide (Fe
2O
3) and analytical pure cobalt sesquioxide (Co
2O
3), in fully ball milling is packed alumina crucible into, carry out synthesizing in advance, again through technological processs such as moulding, preparation BFCT ceramics sample.
Described ball milling is medium with the dehydrated alcohol.
Technology of the present invention is simple, and the oxide compound that adopts existing solid-phase sintering process and market to buy is a raw material, by add two kinds of perovskite-like magnet units in three layers of perovskite ferroelectric materials, has prepared many iron property ceramics sample of laminate structure.
The present invention has effect: (1) has reduced the preparation temperature of many iron pottery; (2) compatible mutually with existing liquid process; (3) sample class calcium titanium layer is arranged and is imitated to orderly; (4) material has good ferroelectricity and ferromegnetism under the greenhouse, the remnant polarization (2P of the stupalith that the present invention forms
r) be～13 μ C/cm
2Suitable with the ferroelectric properties of BFTO sample, its residual magnetization rate exceeds nearly 3000 times for～7.8memu/g than BFTO; (5) simple, the good stability of technology; (6) sintering temperature is low, all raw materials are all nontoxic, has more environment compatibility.
Description of drawings
Fig. 1 is the X ray figure of sample in the embodiment of the invention.
Fig. 2 is a sample stereoscan photograph in the embodiment of the invention.
Fig. 3 is a sample transmission electron microscope photo in the embodiment of the invention.
Fig. 4 is a sample ferroelectric properties measuring result in the embodiment of the invention.
Fig. 5 is magnetic sample performance measurement result in the embodiment of the invention.
Embodiment
Preparation process and condition that embodiment adopts:
(1) preparation of sample raw material:
1) selects analytical pure bismuth oxide (Bi for use
2O
3), analytical pure ferric oxide (Fe
2O
3), analytical pure cobalt sesquioxide (Co
2O
3) and spectroscopically pure titanium oxide (TiO
2) be raw material, raw material all adopts Shanghai chemical reagents corporation product, and raw material toasted 8 hours under 110 ℃ of temperature in baking oven earlier before taking by weighing.
2) preparation of BTO powder: is medium with the bismuth oxide and the titanium oxide (shown in the table 1) that weigh up with the dehydrated alcohol with anhydrous described ball milling, mix the back oven dry through 24 hours ball millings, pack in the alumina crucible, compress gently, in air, respectively under the temperature of 760 ℃, 780 ℃ and 800 ℃, carry out the synthetic of 8 hours, 16 hours and 24 hours.All carry out ball milling and oven dry processing after each synthesizing, the ball milling time is 24 hours, preparation BTO powdered sample.
Table (1) BTO raw material
| Nomenclature of drug | Molecular weight | The charge calculation process | The actual weight that takes by weighing |
| ??Bi 2O 3 | ??465.96 | ??465.96×(1/16)×(1/2)×4/99％(g) | ??67.6579g |
| ??TiO 2 | ??79.87 | ??79.87×(1/16)×1×3/99.9％(g) | ??14.9906g |
(2) preparation of BFCT sample:
1) raw material takes by weighing: take by weighing analytical pure bismuth oxide (Bi by stoicheiometry
2O
3), analytical pure ferric oxide (Fe
2O
3), analytical pure cobalt sesquioxide (Co
2O
3) and the BTO powdered sample, concrete weight is as table (2).
Table (2) BFCT raw material
| Nomenclature of drug | Molecular weight | The charge calculation process | The actual weight that takes by weighing |
| ??BIT | ??1171.53 | ??15(g) | ??15(g) |
| ??Bi 2O 3 | ??465.96 | ??465.96×(1/2)×15/1171.53(g) | ??2.9830(g) |
| ??Co 2O 3 | ??165.86 | ??165.86×(1/4)×15/1171.53(g) | ??0.5309(g) |
| ??Fe 2O 3 | ??159.69 | ??159.96×(1/4)×15/1171.53(g) | ??0.5120(g) |
2) ball milling and pre-synthetic: with the analytical pure bismuth oxide (Bi that weighs up
2O
3), analytical pure ferric oxide (Fe
2O
3), analytical pure cobalt sesquioxide (Co
2O
3) and the BTO powder be medium with the dehydrated alcohol with anhydrous described ball milling, mix the back oven dry through 24 hours ball millings, in the alumina crucible of packing into, compress gently, 640 ℃ of pre-synthesizing 8 hours, all carry out ball milling and oven dry processing after pre-synthesizing in air, the ball milling time is 24 hours.
3) sample moulding, plastic removal: add 5wt% (concentration is the polyvinyl alcohol solution of 10wt%), at the forming under the pressure of～15MPa, make the right cylinder sample, sample size is
12mm * 2mm.With the plastic removal 5 hours under 500 ℃ of temperature of the sample base substrate after the moulding.
4) BFCT ceramic post sintering: the sample base substrate that will cross through plastic removal was 850 ℃ sintering temperature 4 hours.
(3) preparation of BFCT measure sample:
The sample that sinters is carried out surface treatment and attenuate, and it is about 0.5mm that microtexture, dielectric properties and magnetic property measurement reduce to thickness; The thickness of sample that ferroelectric properties is measured reduces to about 0.2mm; Reduce the generation silver electrode to being used for sample that dielectric properties and ferroelectric properties measure with the silver suboxide slurry, electrode size divides and is in addition,
8mm and
About 1mm.
(4) to the BFCT sample measurement condition for preparing be:
With X-ray diffractometer (the Japanese Bruker D8 of company type) sample behind the sintering is carried out structural analysis.With scanning electronic microscope (Dutch Philips company, XL 30ESEM type) and high resolving power transmission electron microscope (Japanese HITACHI company, the H-9000NAR type) surface topography of observation sample and the atomic structure of sample mutually.Vibrating sample magnetometer (EV7 of U.S. ADE Co. type), the magnetic performance of measure sample.Ferroelectric properties with ferroelectric properties survey meter (Precision LC type, Radiant Technologies company) measure sample.
(5) BFCT sample measurement conclusion:
1) sample class calcium titanium layer is arranged and is imitated to orderly; 2) material has good ferroelectricity and ferromegnetism under the greenhouse, the remnant polarization (2P of sample
r) be about 13 μ C/cm
2Suitable with the ferroelectric properties of BFTO sample, its residual magnetization rate is about 7.8memu/g and exceeds nearly 3000 times than BFTO.
Claims (5)
1, a kind of laminate structure ferrotianium cobalt acid bismuth stupalith with multi-ferrum property, its molecular structural formula is: Bi
5Fe
0.5Co
0.5Ti
3O
15
2, a kind of preparation method who has the laminate structure ferrotianium cobalt acid bismuth stupalith of multi-ferrum property according to claim 1 is characterized in that Bi
4Ti
3O
12And BiCoO
3Implant BiFeO
3The middle Bi that forms
5Fe
0.5Co
0.5Ti
3O
15
3, according to the described preparation method of claim 2, it is characterized in that with Bi with laminate structure ferrotianium cobalt acid bismuth stupalith of multi-ferrum property
2O
3And TiO
2Be raw material, under 760～800 ℃ of conditions, synthesize Bi
4Ti
3O
12
4, according to the described preparation method of claim 2, it is characterized in that Bi with laminate structure ferrotianium cobalt acid bismuth stupalith of multi-ferrum property
4Ti
3O
12Powder adds Bi
2O
3, Fe
2O
3And Co
2O
3, carry out synthesizing in advance in the alumina crucible of behind abundant ball milling, packing into, again through moulding, make Bi
5Fe
0.5Co
0.5Ti
3O
15Stupalith.
5,, be medium with the dehydrated alcohol when it is characterized in that described ball milling according to the preparation method of the described laminate structure ferrotianium cobalt acid bismuth stupalith with multi-ferrum property of claim 4.
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|---|---|---|---|
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|---|---|---|---|
| CN2009101822591A CN101607818B (en) | 2009-07-06 | 2009-07-06 | Multiferroic ferrotitanium bismuth cobaltates ceramic material with laminated structure and preparation method thereof |
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| CN101607818B CN101607818B (en) | 2012-05-23 |
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