CN101913867A - Low-frequency multiferroic particle magnetic-electric composite material and preparation method thereof - Google Patents

Low-frequency multiferroic particle magnetic-electric composite material and preparation method thereof Download PDF

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CN101913867A
CN101913867A CN 201010227794 CN201010227794A CN101913867A CN 101913867 A CN101913867 A CN 101913867A CN 201010227794 CN201010227794 CN 201010227794 CN 201010227794 A CN201010227794 A CN 201010227794A CN 101913867 A CN101913867 A CN 101913867A
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multiferroic
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周云
姚雪灿
李同伟
张金仓
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University of Shanghai for Science and Technology
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Abstract

The invention relates to a lead-free nontoxic low-frequency multiferroic nanoparticle magnetic-electric composite material and a preparation method thereof. The low-frequency multiferroic nanoparticle magnetic-electric composite material has magnetic-electric coupling effect. The low-frequency multiferroic nanoparticle magnetic-electric composite material has a chemical formula of xCoFe2O4-(1-x)[0.948(K0.5Na0.5)NbO3-0.052LiSbO3], wherein the optimal mol doping quantity x is 0.2-0.4mol. The parent phase of the composite particle material is 0.948(K0.5Na0.5)NbO3-0.052LiSbO3 with ferroelectricity, which is prepared by using a traditional solid phase method, and the doping phase thereof is a nanoparticle CoFe2O4 with ferroelectricity, which is prepared by using a sol-gel method. The multiferroic particle magnetic-electric composite material has the characteristics of better magnetic-electric coupling property, higher hardness, durability, and the like compared with the similar lead-free particle composite materials; and the preparation method is simple, low in the requirement on production equipment, and easy to massive production. The multiferroic particle magnetic-electric composite material has better ferroelectricity and stronger ferromagnetism and magnetic-electric coupling property, obtains wide application prospect in the fields of a sensor, a capacitor, a magnetic-electric storage, and the like, and achieves important function on the aspect of basic physics research.

Description

A kind of low-frequency multiferroic particle magnetic-electric composite material and preparation method thereof
Technical field
The present invention relates to a kind of unleaded nontoxic many iron of low frequency property nano particle magnetic electric compound material and preparation method thereof with magneto-electric coupled effect.
Background technology
In the modern life and production of device miniatureization, the diversification of demand, more and more exigence possesses multi-functional material simultaneously, and multi-ferroic material is exactly quasi-representative representative wherein.Multi-ferroic material possesses multiple magnetic such as ferroelectric, ferromagnetic simultaneously, and because the coupling between the different iron, and have new performance such as magnetoelectric effect, opened up the range of application of ferroic material greatly.Magnetoelectric effect is meant and applies the effect that magnetic field causes that electropolarization changes, perhaps applies the effect that electric field causes that magnetic polarization changes.The magnetoelectricity voltage coupling coefficient is an important indicator of the magneto-electric coupled effect of exosyndrome material, and it is defined as α E=dE/dH, wherein, E is the electric field output of material, H is the external magnetic field that is applied.The development that is found to be of magneto-electric coupled effect provides huge application potential based on technology such as the novel information stores processor of ferroelectric-integrated effect of magnetic and magnetoelectricity devices.
At present, the material with magnetoelectric effect can be divided into three major types, comprises single-phase compound multi-ferroic material, multiphase granules mixing multi-ferroic material and stratiform multi-ferroic material.General matrix material has the magnetoelectric effect more much higher than single-phase compound, and the bigger value of magnetic-electric coefficient also has only 60 μ Vcm in the monophase materials of report at present -1Oe -1, so matrix material is the emphasis that people research and develop always.First magnetic electric compound material was in the news out in the seventies in 20th century, was with piezoelectric BaTiO 3With piezomagnetic material CoFe 2O 4Particle be combined with each other and form many iron of biphase property magnetoelectric material.Subsequently, similarly such as Co 0.9Cd 0.1Fe 2O 4/ PZT, CoFe 2O 4/ BaTiO 3, Ni 0.8Zn 0.2Fe 2O 4/ Sr 0.5Ba 0.5Nb 2O 6, NiFe 2O 4/ Ba 0.8Sr 0.2TiO 3And Bi 0.8La 0.2FeO 3/ CoFe 2O 4All be synthesized out and obtain concrete research Deng magnetoelectric material.But mostly contain lead as harmful matter in these multiphase granules mixing multi-ferroic materials, environmental pollution is serious, is unfavorable for long-range consideration.The oxide raw material of the Ba element in the other multiphase granules mixing multi-ferroic material also is a toxic substance, is unfavorable for industrial mass production.The magnetoelectricity voltage coefficient of magnetic electric compound material rectangular sheet when the about 60KHz of single order longitudinal resonance frequency under the longitudinal coupled mode of Chinese patent ZL03132167.4 report also reached 8.7V/ (cmOe).Although the magnetoelectric effect of the structure of these magnetic electric compound materials is improved largely, their operating frequency is higher, and this makes the loss of energy in coupling process bigger, thereby has reduced magneto-electric coupled effciency of energy transfer.The stratiform magnetic electric compound material is with respect to before particulate composite, the resistivity that has overcome system in the past is low, is not easy weakness such as polarization, and magnetic electricity performance has huge raising, break through to V/ (cmOe) rank from mV/ (cmOe) rank, can be described as the quantum leap in the magnetic electric compound material preparation.But stratified composite often uses resene glue with ferroelectric phase and ferromagnetic bonding being in the same place in compound, so come off easily and wear out, is difficult for preserving and using for a long time, often is restricted in actual use.In addition, the piezoelectric phase material that most matrix material adopted all contains lead, and this can bring very big pollution to environment.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of nontoxic, and magneto-electric coupled coefficient is better, and is durable in use, the complex phase nano particle mixing multi-ferroic material of working under low operating frequency.
Cobalt ferrite (CoFe 2O 4) be well-known magneticsubstance with spinel structure, it has the characteristic of high resistivity and high piezomagnetic coefficient.Although Pb-based lanthanumdoped zirconate titanates (Pb (Zr, Ti) O 3) possess higher piezo-electric modulus than general piezoelectric, still from the angle of environmental protection, be badly in need of the new material of development in order to substitute the plumbiferous piezoelectric type material of this class.Potassium-sodium niobate base class piezoelectric, especially 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3(KNN-LS5.2) unleaded nontoxic piezoelectric ceramics is substitute of ideal very, and it at room temperature shows high spontaneous polarization, high-k and high tension electricity coefficient, its k 33～62% and d 33～265pC/N.
For achieving the above object, the present invention adopts following technical scheme.
The magnetoelectricity particulate composite is by 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3Ferroelectric blapharoplast and the CoFe that is uniformly distributed in wherein 2O 4The ferromagnetic nano particle constitutes, wherein CoFe 2O 4Molar content in matrix material is between 0.1～0.5.Described CoFe 2O 4In the optimization molar content in matrix material is between 0.2～0.4.The preparation technology of parent is a process for solid phase synthesis, and it is collosol and gel spontaneous combustion method for preparation technology mutually that nano particle mixes.This magnetoelectricity nano particle composite material is made by the raw material of K, Na, Nb, Li, Sb, Co, Fe metallic element, described starting material are oxide compound and the inorganic salt that contain K, Na, Nb, Li, Sb, Co, Fe metallic element, and do not contain the oxide compound of harmful elements Pb and toxic substance Ba.
Concrete preparation method with complex phase nano particle mixing multi-ferroic material of magneto-electric coupled effect provided by the invention comprises the steps:
Prepare ferromagnetic phase nano particle CoFe 2O 4Powder:
Raw material adopts Xiao Suangu [Co (NO 3) 26H 2O], iron nitrate [Fe (NO 3) 39H 2O] and citric acid [C 6H 8O 7H 2O].The primary process of configuration is: at first according to the CoFe that sets 2O 4Stoichiometric ratio take by weighing an amount of Xiao Suangu and iron nitrate, then with citric acid by required weighing, be dissolved in the deionized water, solution is colourless, pH value 1～2.The citric acid solution that will before prepare is heated to about 35～45 ℃ again, two kinds of nitrate are dissolved in the citric acid solution, and to adopt quadrol is intercalating agent that the amount of interpolation is getting final product near 7 with the pH value of solution.Make the fixedly presoma of component of its complexing formation one by adding intercalating agent, wherein citric acid is as complexing agent.The consumption standard of citric acid is defined as: the amount of substance of citric acid should with the Fe of solute in the solution 3+With Co 2+The positively charged ion total mole number equates.Then will continue stirred solution about half hour, and at last solution be inserted in the porcelain unit ware, and on electric furnace, heat spontaneous combustion, form the cobalt ferrite nano particle of black.In order to obtain high-quality CoFe 2O 4Particle, we put into stove with it again, are warmed up to 750～850 ℃, are incubated 2～4 hours, and naturally cool to room temperature.
Preparation ferroelectric phase parent 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3:
Raw material adopts carbonate and the oxide compound that contains potassium metal, sodium, lithium, niobium and antimony.The primary process of preparation is: at first raw material salt of wormwood (K 2CO 3), yellow soda ash (Na 2CO 3), Quilonum Retard (Li 2CO 3), niobium oxides (Nb 2O 5) and weisspiessglanz (Sb 2O 5) 200～300 ℃ of dryings, then according to the 0.948 (K that sets 0.5Na 0.5) NbO 3-0.052LiSbO 3Stoichiometric ratio take by weighing an amount of salt of wormwood, yellow soda ash, Quilonum Retard, niobium oxides and weisspiessglanz respectively, secondly load weighted salt of wormwood, yellow soda ash, Quilonum Retard, niobium oxides and weisspiessglanz were ground in dehydrated alcohol 10～12 hours, then 850 ℃ of calcinings 2～4 hours, (moulding pressure is 10～14MPa) to carry out forming operation at last, then 1050 ℃ of calcinings 6～10 hours, grind afterwards, with standby;
The preparation of composite particulate material:
Ferroelectric phase 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3With ferromagnetic CoFe mutually 2O 4Carry out weighing according to a certain percentage, mix, grind, (moulding pressure is 10～14MPa), calcines 4～6 hours down at 900～1000 ℃ at last, can obtain xCoFe to carry out forming operation then 2O 4-(1-x) 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3The nano particle magnetic electric compound material.
Advantage of the present invention and effect: the nano particle composite material durable with magneto-electric coupled effect of the present invention, sample instability in the stratiform of invention or the bar-shaped magnetic electric compound material before can solving, problem such as come off easily.Magnetic electric compound material with the nano particle composite material of magneto-electric coupled effect and invention before of the present invention compares, biggest advantage is not contain harmful chemical element Pb, and do not contain the Ba element, because containing the oxide raw material major part of Ba element all is toxic substance, industrial difficult preparation.The present invention is extensive use of more environmental protection, and is safer.Nano particle composite material operating frequency with magneto-electric coupled effect of the present invention is lower, and bias magnetic field is lower, and magneto-electric coupled bigger in similar no lead composite material, practicality is stronger.
Description of drawings
Fig. 1 is the variation relation of example magnetoelectricity voltage coefficient with resonant frequency (Frequency).
Fig. 2 be frequency under 1kHz example magnetoelectricity voltage coefficient with direct current biasing magnetic field (H Bias) variation relation.
Embodiment
Following description is to specify of the present invention, should not regard limitation of the invention as.
Molecular formula with complex phase nano particle composite material of magneto-electric coupled effect of the present invention is xCoFe 2O 4-(1-x) [0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3], x=0.3mol wherein.This complex phase nano particle mixing multi-ferroic material principal phase is 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3, mixing is CoFe mutually 2O 4This complex phase nano particle mixing multi-ferroic material is made by the raw material of metallic element, and described starting material are oxide compound and the inorganic salt that contain K, Na, Nb, Li, Sb, Co, Fe metallic element.The making processes of this complex phase nano particle mixing multi-ferroic material comprises selected composition; prepare the principal phase composition respectively and mix composition, at last the principal phase composition with mix composition and mix, grind, burn till step, wherein; the employing agate is a grinding element, and dehydrated alcohol is a grinding medium.
The step for preparing above-mentioned complex phase nano particle mixing multi-ferroic material is:
Prepare ferromagnetic phase nano particle CoFe 2O 4Powder:
Raw material adopts Xiao Suangu [Co (NO 3) 26H 2O], iron nitrate [Fe (NO 3) 39H 2O] and citric acid [C 6H 8O 7H 2O].The primary process of configuration is: at first according to the CoFe that sets 2O 4Stoichiometric ratio take by weighing an amount of Xiao Suangu and iron nitrate, then with citric acid by required weighing, be dissolved in the deionized water, solution is colourless, the pH value is 2.The citric acid solution that will before prepare is heated to 45 ℃ again, two kinds of nitrate are dissolved in the citric acid solution, and to adopt quadrol is intercalating agent, and the amount of interpolation is 7 to get final product with the pH value of solution; Make the fixedly presoma of component of its complexing formation one by adding intercalating agent, wherein citric acid is as complexing agent.The consumption standard of citric acid is defined as: the amount of substance of citric acid equates with the total mole number of solute in the solution.Then will continue stirred solution about half hour, and at last solution be inserted in the porcelain unit ware, and on electric furnace, heat spontaneous combustion, form the cobalt ferrite nano particle of black.In order to obtain high-quality CoFe 2O 4Particle, we put it in the stove again, are warmed up to 850 ℃, are incubated 2 hours, and naturally cool to room temperature.
Preparation ferroelectric phase parent 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3:
Raw material adopts carbonate and the oxide compound that contains potassium metal, sodium, lithium, niobium and antimony.The primary process of preparation is: at first raw material salt of wormwood (K 2CO 3), yellow soda ash (Na 2CO 3), Quilonum Retard (Li 2CO 3), niobium oxides (Nb 2O 5) and weisspiessglanz (Sb 2O 5) 300 ℃ of dry for some time, then according to the 0.948 (K that sets 0.5Na 0.5) NbO 3-0.052LiSbO 3Stoichiometric ratio take by weighing an amount of salt of wormwood, yellow soda ash, Quilonum Retard, niobium oxides and weisspiessglanz respectively, secondly load weighted salt of wormwood, yellow soda ash, Quilonum Retard, niobium oxides and weisspiessglanz were ground in dehydrated alcohol 10 hours, then 850 ℃ of calcinings 2 hours, carry out column forming operation (moulding pressure is 12MPa) at last, then 1050 ℃ of calcinings 8 hours, grind afterwards, with standby;
The preparation of composite particulate material:
Ferroelectric phase 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3With ferromagnetic CoFe mutually 2O 4Carry out weighing according to a certain percentage, mix, grind, carry out column forming operation (moulding pressure is 12MPa) then, calcined 4 hours down at 950 ℃ at last, can obtain 0.3CoFe 2O 4-0.7[0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3] the nano particle magnetic electric compound material.

Claims (3)

1. a low-frequency multiferroic particle magnetic-electric composite material is characterized in that, this magnetoelectricity particulate composite is by 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3Ferroelectric blapharoplast and the CoFe that is uniformly distributed in wherein 2O 4The ferromagnetic nano particle constitutes, wherein CoFe 2O 4Molar content in matrix material is at 0.1～0.5mol.
2. low-frequency multiferroic particle magnetic-electric composite material according to claim 1 is characterized in that described CoFe 2O 4Molar content in matrix material is 0.2～0.4mol.
3. the preparation method of low-frequency multiferroic particle magnetic-electric composite material according to claim 1 is characterized in that this method has following technological process and step:
A. prepare ferromagnetic phase nano particle CoFe 2O 4Powder: according to CoFe 2O 4Stoichiometric ratio take by weighing Xiao Suangu and iron nitrate, by the mole number of citric acid with wait to join the Fe of solute in the solution 3+With Co 2+The positively charged ion total mole number equates to take by weighing citric acid, then citric acid is dissolved in the deionized water pH value 1～2, citric acid solution is heated to 35～45 ℃ again, two kinds of nitrate are dissolved in the citric acid solution, and to adopt quadrol be intercalating agent that the amount of interpolation is 7 to get final product with the pH value of solution; Then continue stirred solution half hour; Again solution is inserted in the porcelain unit ware, and on electric furnace, heat spontaneous combustion, form the cobalt ferrite nano particle of black; Put it into again in the stove, be warmed up to 750～850 ℃, be incubated 2～4 hours, and naturally cool to room temperature;
B. prepare ferroelectric phase parent 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3: with salt of wormwood, yellow soda ash, Quilonum Retard, niobium oxides and weisspiessglanz 200～300 ℃ of dryings, according to 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3Stoichiometric ratio take by weighing salt of wormwood, yellow soda ash, Quilonum Retard, niobium oxides and weisspiessglanz respectively, and they are placed on grind 10～12 hours in the dehydrated alcohol, 850 ℃ of calcinings 2～4 hours, carry out forming operation then, moulding pressure is 10～14MPa, and then, grind afterwards, with standby 1050 ℃ of calcinings 6～10 hours;
C. the preparation of composite particulate material: ferroelectric phase 0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3With ferromagnetic CoFe mutually 2O 4According to xCoFe 2O 4-(1-x) [0.948 (K 0.5Na 0.5) NbO 3-0.052LiSbO 3] the stoichiometric ratio weighing, wherein x=0.1～0.5 is mixed subsequently, is ground, and carries out forming operation then, moulding pressure is 10～14MPa, 900～1000 ℃ of down calcinings 4～6 hours, can obtain low-frequency multiferroic particle magnetic-electric composite material at last.
CN 201010227794 2010-07-15 2010-07-15 Low-frequency multiferroic particle magnetic-electric composite material and preparation method thereof Pending CN101913867A (en)

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Cited By (4)

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CN105206710A (en) * 2015-10-22 2015-12-30 重庆科技学院 Preparation method of ferroelectric film with texture
CN107382309A (en) * 2017-08-03 2017-11-24 中南大学 A kind of unleaded Bi0.5Na0.5TiO3Base magnetoelectric ceramic and preparation method thereof
CN108546124A (en) * 2018-05-03 2018-09-18 佛山九陌科技信息咨询有限公司 A kind of preparation method of BCZT based leadless piezoelectric ceramics
CN115231921A (en) * 2022-07-27 2022-10-25 贵州大学 Ferromagnetic coupling material and preparation method thereof

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105206710A (en) * 2015-10-22 2015-12-30 重庆科技学院 Preparation method of ferroelectric film with texture
CN105206710B (en) * 2015-10-22 2017-04-05 重庆科技学院 The preparation method of the ferroelectric thin film with texture
CN107382309A (en) * 2017-08-03 2017-11-24 中南大学 A kind of unleaded Bi0.5Na0.5TiO3Base magnetoelectric ceramic and preparation method thereof
CN107382309B (en) * 2017-08-03 2020-08-04 中南大学 Lead-free Bi0.5Na0.5TiO3Base magnetic electric composite ceramic and preparation method thereof
CN108546124A (en) * 2018-05-03 2018-09-18 佛山九陌科技信息咨询有限公司 A kind of preparation method of BCZT based leadless piezoelectric ceramics
CN108546124B (en) * 2018-05-03 2021-07-30 景德镇市鑫惠康电子有限责任公司 Preparation method of BCZT-based lead-free piezoelectric ceramic
CN115231921A (en) * 2022-07-27 2022-10-25 贵州大学 Ferromagnetic coupling material and preparation method thereof
CN115231921B (en) * 2022-07-27 2023-03-31 贵州大学 Ferromagnetic coupling material and preparation method thereof

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Application publication date: 20101215