CN101704669A - Layered structure ferrotitanium lanthanum bismuth cobaltate ceramic with multiferroic and preparation method thereof - Google Patents

Layered structure ferrotitanium lanthanum bismuth cobaltate ceramic with multiferroic and preparation method thereof Download PDF

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CN101704669A
CN101704669A CN200910232041A CN200910232041A CN101704669A CN 101704669 A CN101704669 A CN 101704669A CN 200910232041 A CN200910232041 A CN 200910232041A CN 200910232041 A CN200910232041 A CN 200910232041A CN 101704669 A CN101704669 A CN 101704669A
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陈小兵
毛翔宇
王伟
陆亚林
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Abstract

The invention relates to a layered structure ferrotitanium lanthanum bismuth cobaltate ceramic with multiferroic and a preparation method thereof, relating to the technical field of oxide ceramic material preparation. The method comprises the following steps: firstly preparing Bi3.25L0.75Ti3O15 powder, then implanting BiCoO3 and BiFeO3 in Bi3.25L0.75Ti3O15 to form Bi4.25L0.75Fe0.5Co0.5Ti3O15 ceramic. In the obtained BLFCT sample, the octahedral arrangement of Fe-O and Co-O is relatively orderly so that the local coupling between Fe-O-Co and La-O-Co/Fe can be obtained and the ferroelectric property and magnetic property of the sample can be improved. The ceramic of the invention has simple and reasonable technology and good compatibility with the current technology, and the sample preparation temperature is much lower than the preparation temperature of the current technology so as to greatly reduce the energy consumption, thus the ceramic is applicable to industrial production.

Description

Has laminate structure ferrotitanium lanthanum bismuth cobaltate ceramic of multi-ferrum property and preparation method thereof
Technical field
The present invention relates to the oxide ceramic material preparing technical field.
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, has simple uhligite ABO 3The BiFeO of type structure 3Be a kind of unleaded environmentally friendly material, have ferroelectric Curie temperature and antiferromagnetic Neel temperature, thereby receive much concern far above room temperature.However, the BFO material, no matter pottery and film morphology, the shortcoming that all has some to be difficult to overcome, big as dielectric loss, leakage current is higher, ferroelectric residual polarization is less, big and its magnetic spin structure heterogeneous of coercive field etc.In recent years, although BFO has obtained extensive studies, because the shortcoming of self can't must be used in practical devices.
At multi-iron material laminate perovskite material,, obtain people and pay attention to widely owing to contain the Bi-O layer in the structure and work to do the space charge storehouse and insulation layer can effectively reduce the leakage current of material.Ferrotianium acid bismuth (Bi 5FeTi 3O 15, BFTO) being a kind of typical laminated perovskite magnetodielectric material, 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.
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 (as Fe: Co=1: in the time of 1, the coupling probability maximum of Fe-O-Co) between Fe, the Co ion, this being coupled with may show as ferromegnetism.In BTO research, find in addition, replace BTO sample A position Bi ion (BLT-0.75), can effectively reduce the oxygen vacancy concentration in the sample, improve the ferroelectric properties of sample with the La series elements.Experimental study shows: over-all properties the best of sample when the La doping is 0.75.Studies show that for many ferroelectric materials not only the ferromagnetic energy of B position coupling can improvement sample simultaneously, can improve the ferromagnetic property of sample equally by the coupling of A position La series elements.The application introduces magnetosphere (BiFeO based on the constructional feature of laminated perovskite multi-iron material in the BLT-0.75 sample that has prepared 3, BiCoO 3, Fe: Co=1: 1), preparation Bi 4.25L 0.75Fe 0.5Co 0.5Ti 3O 15(BLFCT), also can be described as with the preparation of improved solid-phase sintering process, by the BFTO sample is carried out A, the B position is implemented the novel multi-ferroic material that mixes and form simultaneously.About this material of BLFCT, we do not see the document of related work and the report of patent at present.
Summary of the invention
The objective of the invention is to provide a kind of when having laminated perovskite structure, have ferroelectric, ferromagnetic novel many iron of magnetoelectricity pottery.
Laminate structure ferrotitanium lanthanum bismuth cobaltate ceramic with multi-ferrum property is ceramic Bi 4. 25L 0.75Fe 0.5Co 0.5Ti 3O 15
Another purpose of the present invention provides above preparation methods:
Prepare Bi earlier 3.25L 0.75Ti 3O 15Powder is again with BiCoO 3And BiFeO 3Implant Bi 3. 25L 0.75Ti 3O 15The ceramic Bi of middle formation 4.25L 0.75Fe 0.5Co 0.5Ti 3O 15
Preparation technology of the present invention is from ceramic Bi 4.25L 0.75Fe 0.5Co 0.5Ti 3O 15(BLFCT) structure is set out, earlier preparation Bi 3.25L 0.75Ti 3O 15(BLT) powder is again with BiCoO 3And BiFeO 3Implant among the BLT and form BLFCT.Therefore in obtaining the BLFCT sample, the octahedra arrangement of Fe-O and Co-O is comparatively orderly, thereby the part obtains the coupling between Fe-O-Co and the La-O-Co/Fe, thereby improves the ferroelectric and magnetic property of sample.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.
Technical scheme of the present invention is to be divided into for two steps: the preparation of (1) BLT powder; (2) preparation of BLFCT ceramics sample.
(1) preparation of BLT powder: adopt traditional solid-phase sintering process, it is characterized in that with analytical pure bismuth oxide (Bi 2O 3), lanthanum trioxide (LaO 2) and spectroscopically pure titanium oxide (TiO 2) be raw material, take by weighing raw material by stoicheiometry, carry out repeatedly synthetic at 760 ℃～800 ℃.
Concrete scheme is: with analytical pure bismuth oxide, lanthanum trioxide and titanium oxide is that medium carries out ball milling with the dehydrated alcohol, mix the back oven dry through 24 hours ball millings, pack in the alumina crucible, 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 respectively.
(2) preparation of BLFCT: with BiCoO 3And BiFeO 3Implant Bi 3.25L 0.75Ti 3O 15The ceramic Bi of middle formation 4.25L 0.75Fe 0.5Co 0.5Ti 3O 15Method be: with Bi 3.25L 0.75Ti 3O 15Powder adds analytical pure bismuth oxide (Bi 2O 3), analytical pure ferric oxide (Fe 2O 3) and analytical pure cobalt sesquioxide (Co 2O 3), behind ball milling, carry out in the alumina crucible of packing into synthesizing in advance, through moulding, plastic removal, sintering process process, prepare ceramic Bi again 4.25L 0.75Fe 0.5Co 0.5Ti 3O 15
Described ball milling is medium with the dehydrated alcohol.
Described moulding, plastic removal technology are: add polyvinyl alcohol solution in pre-synthetic materials, at the condition compacted under of pressure≤15MPa, with the plastic removal 5 hours under 500 ℃ of temperature of the sample base substrate after the moulding.
Described sintering is: the sample base substrate that will cross through plastic removal was 840 ℃ sintering temperature 4 hours.
Technology of the present invention is simple, the oxide compound (Shanghai traditional Chinese medicines group) that adopts existing solid-phase sintering process and market to buy is a raw material, by in three layers of perovskite ferroelectric materials, adding two kinds of perovskite-like magnet units, prepared many iron property ceramics sample of laminate structure.
The present invention has effect: the preparation temperature that 1, has reduced 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, when sample is 150kV/cm at the measurement electric field, and remnant polarization (2P r) be～11.7 μ C/cm 2The ferroelectric properties that obviously is better than the BFTO sample, sample residual magnetization rate are that 12.5memu/g exceeds nearly 5000 times than BFTO sample; 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 ferroelectric properties measuring result in the embodiment of the invention;
Fig. 4 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 lanthanum trioxide (LaO 2), 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 BLT powder: with bismuth oxide, lanthanum trioxide and the titanium oxide (shown in the table 1) that weighs up is that medium carries out ball milling with the dehydrated alcohol, 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 BLT powdered sample.
Table 1: preparation BLT raw material
Nomenclature of drug Molecular weight The materials calculation formula The materials quality
??Bi 2O 3 ??465.96 ??465.96×(1/16)×(1/2)×3.25/99％×1.15(g) ??54.9724(g)
??La 2O 3 ??325.81 ??325.96×(1/16)×(1/2)×0.75/99％(g) ??7.7133(g)
??TiO 2 ??79.87 ??79.87×(1/16)×1×3/99.9％(g) ??14.9906(g)
(2) preparation of BLFCT 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) (3).
Table 2: preparation BiFe 0.5Co 0.5O 3Raw material
Nomenclature of drug Molecular weight The materials calculation formula The materials quality
??Bi2O3 ??465.96 ??465.96×(1/4)×(1/2)/99％(g) ??58.8333(g)
??Co2O3 ??165.86 ??165.86×(1/4)×(1/2)×0.5/99％(g) ??10.4710(g)
??Fe2O3 ??159.69 ??159.69×(1/4)×(1/2)×0.5/99％(g) ??10.0814(g)
Table 3: preparation Bi 4.25L 0.75Fe 0.5Co 0.5Ti 3O 15Raw material
Nomenclature of drug Molecular weight The charge calculation formula The materials quality
??Bi 3.25La 0.75Ti 3O 12 ??1118.97 ??15(g) ??15(g)
??BiFe 0.5Co 0.5O 3 ??314.37 ??314.37×15/1118.97(g) ??4.2142(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 BLT powder be that medium carries out ball milling with the dehydrated alcohol, mix the back oven dry through 24 hours ball millings, in the alumina crucible of packing into, compress gently, in air, pre-synthesizing 8 hours under 640 ℃ of conditions, all carry out ball milling and oven dry processing after pre-synthesizing, the ball milling time is 24 hours.
3) sample moulding, plastic removal: add polyvinyl alcohol solution in pre-synthetic materials, at the condition compacted under of pressure≤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) BLFCT ceramic post sintering: the sample base substrate that will cross through plastic removal was 840 ℃ 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,
Figure G2009102320412D0000061
8mm and
Figure G2009102320412D0000062
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.Obtain Fig. 1,2,3,4.
As can be seen from Fig. 1:
The BLFCT sample is the ceramics sample of single perovskite structure, does not find second phase.
As can be seen from Fig. 2:
The crystal grain of sample is sheet, and the density of sample is better, and obviously the cavity does not occur.
As can be seen from Fig. 3:
Under the normal temperature, the BLFCT sample demonstrates good ferroelectric, is under the 150kV/cm measuring electric field, the residual polarization (2P of sample r) be 11.7 μ C/cm 2Coercive field is 105kV/cm.
As can be seen from Fig. 4:
Under the normal temperature, the BLFCT sample demonstrates ferroelectricity, the residual polarization (2M of sample r) be 12.5memu/g coercive field (2H c) be 365Oe.

Claims (8)

1. the laminate structure ferrotitanium lanthanum bismuth cobaltate ceramic that has multi-ferrum property is characterized in that described material is ceramic Bi 4.25L 0.75Fe 0.5Co 0.5Ti 3O 15
2. a preparation method who has the laminate structure ferrotitanium lanthanum bismuth cobaltate ceramic of multi-ferrum property according to claim 1 is characterized in that preparation Bi earlier 3.25L 0.75Ti 3O 15Powder is again with BiCoO 3And BiFeO 3Implant Bi 3.25L 0.75Ti 3O 15The ceramic Bi of middle formation 4.25L 0.75Fe 0.5Co 0.5Ti 3O 15
3. according to the described preparation method of claim 2, it is characterized in that preparing Bi with laminate structure ferrotitanium lanthanum bismuth cobaltate ceramic of multi-ferrum property 3.25L 0.75Ti 3O 15The method of powder is: adopting solid-phase sintering process, is raw material with analytical pure bismuth oxide, lanthanum trioxide and spectroscopically pure titanium oxide, synthesizes at 760 ℃～800 ℃.
4. according to the described preparation method of claim 3 with laminate structure ferrotitanium lanthanum bismuth cobaltate ceramic of multi-ferrum property, it is characterized in that with analytical pure bismuth oxide, lanthanum trioxide and titanium oxide being that medium carries out ball milling with the dehydrated alcohol, mix the back oven dry through 24 hours ball millings, pack in the alumina crucible, 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 respectively.
5. according to claim 2 or 3 described preparation methods, it is characterized in that BiCoO with laminate structure ferrotitanium lanthanum bismuth cobaltate ceramic of multi-ferrum property 3And BiFeO 3Implant Bi 3.25L 0.75Ti 3O 15The ceramic Bi of middle formation 4.25L 0.75Fe 0.5Co 0.5Ti 3O 15Method be: with Bi 3.25L 0.75Ti 3O 15Powder adds analytical pure bismuth oxide, analytical pure ferric oxide (Fe 2O 3) and the analytical pure cobalt sesquioxide, behind ball milling, carry out in the alumina crucible of packing into synthesizing in advance, through moulding, plastic removal, sintering process process, prepare ceramic Bi again 4. 25L 0.75Fe 0.5Co 0.5Ti 3O 15
6. according to the described preparation method of claim 5, it is characterized in that described ball milling is medium with the dehydrated alcohol with laminate structure ferrotitanium lanthanum bismuth cobaltate ceramic of multi-ferrum property.
7. according to the described preparation method of claim 5 with laminate structure ferrotitanium lanthanum bismuth cobaltate ceramic of multi-ferrum property, it is characterized in that described moulding, plastic removal technology are: in pre-synthetic materials, add polyvinyl alcohol solution, at the condition compacted under of pressure≤15MPa, with the plastic removal 5 hours under 500 ℃ of temperature of the sample base substrate after the moulding.
8. according to the described preparation method with laminate structure ferrotitanium lanthanum bismuth cobaltate ceramic of multi-ferrum property of claim 5, it is characterized in that described sintering is: the sample base substrate that will cross through plastic removal was 840 ℃ sintering temperature 4 hours.
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CN102167584A (en) * 2010-12-31 2011-08-31 扬州大学 Ferrotitanium bismuth cobaltate ceramic material with five-laminated structure and multiferroic performance and preparation method thereof
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