CN105006329B - A kind of multiferroic liquid and preparation method thereof - Google Patents

A kind of multiferroic liquid and preparation method thereof Download PDF

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CN105006329B
CN105006329B CN201510427302.1A CN201510427302A CN105006329B CN 105006329 B CN105006329 B CN 105006329B CN 201510427302 A CN201510427302 A CN 201510427302A CN 105006329 B CN105006329 B CN 105006329B
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liquid
multiferroic
nano particle
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multiferroic liquid
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CN105006329A (en
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邓小玲
高荣礼
符春林
蔡苇
陈刚
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Jiaxing Dingshan Information Technology Co.,Ltd.
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Chongqing University of Science and Technology
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Abstract

The invention discloses a kind of multiferroic liquid and preparation method, once solving, solid-state multi-ferroic material coercivity is big, is molded that its structure cannot change, magnetoelectric effect is weak, easily by the deficiency of voltage breakdown.The multiferroic liquid is dispersed in the stable suspension formed in the mixing liquid of base fluid and surfactant by the nano particle of the internal magnetoelectricity core shell structure for wrapping up ferroelectric material for magnetic material, magnetic material outer surface.The multiferroic liquid of the present invention not only has ferroelectricity, magnetic, also there is mobility, its coercivity is smaller, different electric fields or magnetic field can be applied to multiferroic liquid as needed to adjust length, the thickness of the nano chain of the composition of the nano particle in multiferroic liquid, so as to adjust the electricity of multiferroic liquid, magnetics, hydrodynamics, optics and the characteristic of acoustic connection.Present invention firstly provides the concept of multiferroic liquid, and preparation method is provided, new research direction has been opened up for the research of multi-ferroic material.

Description

A kind of multiferroic liquid and preparation method thereof
Technical field
The invention belongs to multi-ferroic material field, and in particular to a kind of multiferroic liquid and preparation method thereof.
Background technology
The Schmid of Switzerland in 1994 clearly proposes multi-ferroic material this concept, multi-ferroic material (mutliferroic) refer to the basic performance comprising two kinds and two or more iron in the same phase of material, these iron it is basic Performance includes ferroelectricity (anti-ferroelectricity), ferromagnetism (anti-ferromagnetism, ferrimagnetism) and ferroelasticity.This kind of material is in certain temperature Degree is lower to have spontaneous polarization sequence and spin sequence simultaneously, caused magnetoelectric effect while being exactly them be present, makes multiferroic Body has some special physical properties, has triggered some new, significant physical phenomenons, such as：Under the influence of a magnetic field Produce electric polarization or induction ferroelectric phase transition；Magnetic field or induction ferromagnetic phase transition are produced under electric field action；In Curie temperature iron Magnetic phase transition point nearby produces the mutation of dielectric constant, and multi-ferroic material has turned into the current focus studied in the world.
The same with ferromagnetic material, ferroelectric material can be used for information storage.Due to ferroelectric material have excellent ferroelectricity, The characteristics such as dielectric, pyroelectric, electro-optical characteristic, acousto-optic performance, nonlinear optics, they ferroelectric memory, infrared detector, There is very important application in terms of the solid-state devices such as sensor, surface acoustic wave, integrated optoelectronic device, capacitor, this is also very big Ground has promoted the research and development of ferroelectric material and feroelectronics.Based on the Ferroelectric Random Access Memory of ferroelectric material because its is non- The features such as volatibility and fast reading speed and there is huge application prospect.Ferroelectric material and its application study turn into condensed state One of research topic that physics, Solid State Electronics field are most popular.
At present simultaneously have ferroelectric order and magnetic it is orderly material it is also few, typically have bismuth ferrite (BiFeO3, referred to as BFO), mangaic acid bismuth (BiMnO3, abbreviation BMO), sieve breath salt (NaKC4H4O6.4H2O)、BaFe12O19Deng.Moreover, that studies at present is more Ferroic material is all solid-state, including multiferroic ceramics, multiferroic film, multiferroic monocrystalline etc..There is ferroelectric order simultaneously at present Orderly single-phase material material is few with magnetic, or and these materials are that magnetic is not strong enough, or be exactly that ferroelectricity is weaker, It is exactly Curie temperature than relatively low (only just there is magnetic and ferroelectricity at low temperature).Solid-state multi-ferroic material exist it is following not Foot：1st, the coercivity of solid-state multi-ferroic material is bigger, when with magnetic field or electric field come modulator magnetic or it is ferroelectric when, need The magnetic field wanted or electric field are also just bigger；2. when its magnetoelectric effect is studied, it is found that the weak change of Benefit Transfer is not clear It is aobvious；3. applying electric field greatly easily to damage multi-ferroic material, waste of material is caused；4. multi-ferroic material, which is once molded, to be changed Become.The multi-ferroic material of liquid has not been reported, and does not also have " multiferroic liquid " this concept in the world.Because when Multi-ferroic material is in liquefaction then, and temperature is typically all higher than its ferroelectrie Curie temperature or ferromagnetic Curie temperature, this When multi-ferroic material lost ferroelectricity and (or) ferromagnetism (or ferrimagnetism, anti-ferromagnetism).Therefore, we carry first Go out " multiferroic liquid " this concept, and give its preparation method.
The content of the invention
In order to solve the deficiency of solid-state multi-ferroic material, the invention provides a kind of multiferroic liquid and preparation method thereof.
The present invention is achieved through the following technical solutions：
A kind of multiferroic liquid, including the nano particle of multiferroic, base fluid and surfactant；The nano particle it is interior Portion is magnetic material, and the outer surface of the magnetic material is fully wrapped around by ferroelectric material；The base fluid and the surfactant Mixing liquid is uniformly mixed into, the nano particle, which is dispersed in, forms stable suspension in the mixing liquid.
Further, Li Jing≤20nm of the nano particle.
Further, the nano particle is nanoparticle or nano wire with multiferroic.
Further, the base fluid is water, organic liquid or aqueous organopolysiloxane.
Further, the base fluid is silicone oil, detergent alkylate or Polybutene oil.
Further, the surfactant be oleic acid, aminododecane, fluorine ether acid, laurate, phenyl undecanoic acid at least It is a kind of.
The method for preparing any of the above-described described multiferroic liquid, comprises the following steps：
Prepare base fluid, surfactant and the nano particle of drying；
Base fluid and surfactant are uniformly mixed into mixing liquid, then nano particle is added the appearance equipped with mixing liquid In device, shake container and avoid reuniting, precipitate by nano particle is scattered, sealing container is simultaneously placed on to shake on shaking table and makes multiferroic Nano particle is uniformly dispersed in mixing liquid, so as to the multiferroic liquid that the nano particle volume fraction stablized is V% Body,
Further, the shaking table shake time is more than half an hour.
Further, in order that multiferroic liquid is more stable, the V% is less than 20%.
Further, in order that multiferroic liquid is more stable, the V% is less than 2%.
Beneficial effects of the present invention：
1st, for solid-state multi-iron material because its coercivity is bigger, when with magnetic field or electric field come modulator magnetic or iron Electrically when, it is necessary to field it is bigger.And multiferroic liquid, its coercivity are smaller, due to nanoparticle suspension in a liquid, Nano particle is influenceed by Brownian movement, and liquid is much smaller with respect to for solid to the resistance of nanoparticle movement.Outside Under power effect, nano particle can rotate in a liquid, and its magnetic moment direction or polarised direction can accordingly change, so Afterwards inside solid, crystal grain obviously can not rotate, and resistance is very big.
2nd, for solid-state multi-iron material, when studying its magnetoelectric effect, it is found that magnetoelectric effect is weaker.Apply Change very little when added electric field to magnetic property, or, influence very little when applying magnetic field to its ferroelectric properties.For Multiferroic liquid, each nano particle have ferroelectricity and magnetic, and when applying electric field, nano particle just occurs to turn It is dynamic, its magnetic moment also concomitant rotation；Conversely, when applying magnetic field, nano particle, will be light under magnetic direction due to being magnetic Pine rotates, and polarised direction also changes；As long as applying electric field or the magnetic field of very little, it can just cause magnetic moment direction or polarised direction Rotate.Multiferroic liquid improves magnetoelectric effect.
3rd, for solid-state multi-ferroic material, application electric field is excessive, and solid-state multi-ferroic material is easy to be damaged by electric field breakdown It is bad, and this breakdown is permanent, it is impossible to recover.For multiferroic liquid, after some point is broken down by electric field breakdown, only Power down (magnetic) field is needed, is shaken, then applies electric (magnetic) field again, multiferroic liquid and can is recovered to use.Moreover, multiferroic Liquid only needs the electric field of very little with regard to that can change its polarised direction, therefore is also not easy breakdown.
4th, for solid-state multi-ferroic material, structure cannot change once being molded.And multiferroic liquid, due to liquid Mobility, after applying electric (magnetic) field, it can easily change the length thickness of nano chain.The internal structure of multiferroic liquid It is variable.Need not with when just not to electric (magnetic) field, it is necessary to when apply electric (magnetic) field, can after being finished To go to power down (magnetic) field.And nano chain can arbitrarily be controlled by parameters such as the size of electric (magnetic) field of change, direction, gradients Structure.Such as into photovoltaic cell, using solid-state multi-ferroic material, the thickness of film layer be exactly it is constant, between electrode away from Area from, electrode is all constant；If nano wire, then the length thickness distance of nano wire is all invariable. Using multiferroic liquid, then can by changing the factors such as electric (magnetic) field size direction, come change the length of nano chain, thickness, Distance.
5th, multiferroic liquid, there is magneto-optic effect, refraction effect, these performances not having in solid-state ferroelectric material.
6th, under electric field or magnetic fields, the orientation of electricdomain can only be along close to direction of an electric field in solid-state multi-ferroic material Some orientations, might not be along direction of an electric field, and for ferroelectricity multiferroic liquid, due to ferroelectric nano particle Can freely it rotate in a liquid, therefore the orientation of its electricdomain can be completely along direction of an electric field.
Because multiferroic liquid has ferroelectricity, magnetic and mobility simultaneously, therefore with many unique electricity, magnetic , hydrodynamics, optics and acoustic characteristic.When multiferroic liquid is placed in uniform electric field or the magnetic field of some strength, when it is a branch of partially When the light that shakes passes through, the electric vector of polarised light is poor with that can exist perpendicular to dispatch from foreign news agency field direction absorbing state parallel to dispatch from foreign news agency field direction It is different, thus be optically anisotropic, a series of electrooptic effects such as Faraday effect, birefringence effect will be produced.Multiferroic liquid There is phenomena such as electrical conductivity frequency dispersion, ferroelectricity viscosity in alternating field.It is also possible to multiferroic liquid is controlled by electric field Magnetic, magnetic field can also be applied in turn to change its electrical property.
In a word, present invention firstly provides multiferroic liquid and preparation method is provided, is opened for the research of multi-ferroic material New direction is opened up.And the use of the present invention by magnetic material is core, ferroelectric substance coated magnetic material is what shell formed Nano particle, prepare simply, and the nano particle has ferroelectricity and magnetic simultaneously, also with mobility, while to magnetic (electricity) Field is all very sensitive, makes the multiferroic liquid of the present invention have magnetoelectric effect, compared with the magneto-electric coupled effect of solid-state multi-ferroic material Should be stronger.The material of the multiferroic of the present invention, has certain application value in sensor, air locking etc..
Brief description of the drawings
Fig. 1 is the multiferroic liquid schematic diagram of the present invention；
Fig. 2 be the present invention multiferroic liquid magnetic (electricity) field or magnetic field electric field and meanwhile in the presence of nano particle along magnetic The direction of (electricity) field is arranged in chain；
Fig. 3 is the TEM figures of the multiferroic liquid of CFO-BFO core shell structures；
Fig. 4 is the magnetization curve of CFO-BFO Core-shell Structure Nanoparticles；
Fig. 5 is the magnetization curve for the CFO-BFO core shell structure multiferroic liquid that volume fraction is 2%.
Embodiment
With reference to embodiment and accompanying drawing, the invention will be further described.
A kind of multiferroic liquid, including the nano particle of multiferroic, base fluid and surfactant.The nano particle it is interior Portion forms the core of nano particle, the preferred ferroso-ferric oxide of magnetic material (Fe3O4), Conjugate ferrite for magnetic material (CoFe2O4, write a Chinese character in simplified form CFO) or (γ-Fe2O3(those skilled in the art, which should appreciate that, can also use other magnetic materials)；Institute The outer surface of ferroelectric material is stated by the fully wrapped around shell for forming nano particle of magnetic material, the preferred barium titanate of ferroelectric material (BTO) or lead zirconate titanate (PZT) (those skilled in the art, which should appreciate that, can also use other ferroelectric substances), formed magnetic- The nano particle of the multiferroic of electric core shell structure.The base fluid and the surfactant are uniformly mixed into mixing liquid, described Nano particle, which is dispersed in, forms stable suspension in the mixing liquid.With the nanometer of ferroelectric material coated magnetic material Particle, because ferroelectric material is on the surface of nano particle, it is easy to influenceed by electric field, therefore apply very to multiferroic liquid Small electric field can also have an impact to nano particle.Li Jing≤20nm of the nano particle.The particle diameter of nano particle is smaller more Good, particle diameter is smaller, and because coulomb moves, nano particle is just less likely to occur to precipitate.Conversely, particle diameter is bigger, due to by gravity Effect, is easy for precipitating, it is impossible to form suspension.If particle diameter is big, density also very big base fluid body must be just selected, Gravity is offset with buoyancy, so selection to base fluid is just harsher, and alternative base fluid is with regard to fewer.The nanometer Particle is nanoparticle or nano wire with multiferroic.The base fluid is water, organic liquid or aqueous organopolysiloxane.In order to The multiferroic of multiferroic liquid is characterized, it is necessary to electric field is applied to multiferroic liquid so that the multiferroic in liquid is micro- Grain is polarized.Therefore, base fluid should just select the very poor liquid of electric conductivity, such as grease type close to insulation, should additionally have There is some other performance：Breakdown strength is high, and dielectric loss angle tangent is small, and insulation resistivity is high, and relative dielectric constant is small；Next to that With excellent physical and chemical properties.Such as vapourizing temperature height, flash-point is high, as far as possible fire retardant or non-ignitable；Freezing point is low, suitable viscous Degree and viscosity-temperature profile；Thermal conductivity is big, and specific heat capacity is big；Heat endurance is good, resistance to oxidation；It is inspiratory small under electric field action；It Compatibility between the solid material contacted will get well；Toxicity is low, easily biological-degradable.Also require that source is wide, price is low.Base Liquid is preferably for silicone oil, detergent alkylate or Polybutene oil for being used under high temperature etc..The table that the dielectricity of selection and base fluid matches Face activating agent oleic acid, aminododecane, fluorine ether acid, laurate or phenyl undecanoic acid.Selected surfactant can wrap up The nano particle and can is dissolved in selected base fluid.
The preparation of CFO-BTO magnetic-electric core shell structure multiferroic liquid
1st step：Preparation has ferromagnetic CFO nano particles
By FeCl3·6H2O (0.04mol, 100mL) and Co (NO3)2·6H2O (0.02mol, 100mL) is mixed, and is added NaOH (0.35mol, 500mL), mixed solution then be heated to seethe with excitement, with its quick stirring；Boiling is removed after continuing 1min Natural sedimentation；1mol/L H (NO) is fully used after precipitation3Cleaning is carried out to sediment for solution until pH value is 7；Then will cleaning Products therefrom obtained after the process such as being dehydrated, drying by acetone required for there is ferromagnetic CFO nano particles.
2nd step：CFO-BTO magnetic-electric Core-shell Structure Nanoparticles are prepared with sol-gel process
1) preparation of barium precursor liquid：Appropriate glacial acetic acid is added in barium acetate, is placed in 80 DEG C of thermostat water baths and adds Heat of solution, it is transferred to after cooling in volumetric flask, ethylene glycol ethyl ether constant volume, which is added dropwise, using buret produces Ba precursor liquids.2) titanium precursor The preparation of liquid：Glacial acetic acid and ethylene glycol ethyl ether are added in butyl titanate as mixed solvent, appearance is transferred to after dissolving In measuring bottle, ethylene glycol ethyl ether constant volume is instilled using buret and produces Ti precursor liquids.Ti precursor liquids are added drop-wise in Ba precursor liquids, dripped Appropriate acetylacetone,2,4-pentanedione is added after adding to adjust dissolved adhesiveness, the colloidal sol for producing pure barium titanate through 24 hours after well mixed.If need The colloidal sol of barium titanate doping is prepared, only need to add appropriate La precursor liquids, Nd precursor liquids or Co precursor liquids simultaneously, it is old through 24 hours The colloidal sol of barium titanate doping is produced after change.If necessary, ethanol in proper amount amine can be also added to control the viscosity of colloidal sol.Then will step The CFO magnetic nanoparticles prepared in rapid 1 are added in colloidal sol, and finally the mixture of obtained colloidal sol and particulate is existed Toasted on warm table, being put into batch-type furnace after drying is sintered, and is 900 DEG C in sintering temperature, time 2h.By gained After product is fully ground, the required CFO-BTO nano particles with magnetic-electric core shell structure are obtained.
3rd step：The preparation of CFO-BTO magnetic-electric core shell structure multiferroic liquid
As desired, there are CFO-BTO magnetic-electric Core-shell Structure Nanoparticles to be uniformly dispersed in necessarily certain mass In the silicone oil of concentration.Silicone oil has the characteristics that high-low temperature resistant, chemical stability are good, steam forces down, viscosity is affected by temperature small, is The preferable carrier fluid of multiferroic liquid.But the characteristic of silicone oil water and oil repellence causes will have CFO-BTO magnetic-electric core shell structure to receive Rice grain, which is dispersed in surfactant therein, must have oleophylic performance, and energy coated magnetic particulate, otherwise easily occur Phenomena such as reuniting, settling.From oleic acid as surfactant.
Specially：Configuration particulate volume fraction is 5%, cumulative volume is that 100ml has CFO-BTO magnetic-electric core shell structure Multiferroic liquid, then, required particulate volume is 5ml, and its density is about 6g/cm3, then the quality for needing particulate is 30g；Oil The concentration of acid is 2%, then needs to measure 2ml oleic acid；The volume of silicone oil is 100-5-2=93ml.
First, weigh 30g has CFO-BTO magnetic-electric core shell structure (volume about 5cm3), be added to 2ml oleic acid and In the mixed uniformly mixing liquid of 93ml silicone oil, shaken, prevent nanoparticle agglomerates, precipitation, then liquid is put into sealing In good vial or other containers, carry out shaking 1 hour on shaking table.Then just obtain microsome fraction for 5%, Cumulative volume has CFO-BTO magnetic-electric core shell structure multiferroic liquid for 100ml's.
Fig. 1 is multiferroic liquid schematic diagram, and the black portions in Fig. 1 inside circle, which represent, has magnetic nano particle, Can be CFO, Fe3O4Deng.The grey wrapping portion of black circles outer surface, which represents, has ferroelectric integument, Ke Yishi BTO, PZT etc..Regional Representative's base fluid of grey, can be water, acid, oil, hydrocarbon etc..As shown in figure 1, not to multiferroic liquid When applying electric (magnetic) field, nanoparticle arrangement in multiferroic liquid is random to be in disordered state.
As shown in Fig. 2 apply electric (magnetic) field (or applying direction identical electric field and magnetic field simultaneously) to multiferroic liquid, Along the direction of additional " field ", while there is the nano particle of ferroelectricity and magnetic just to form chain along the direction ordered arrangement of " field " Shape, therefore other properties of multiferroic liquid can be regulated and controled, such as translucency.Therefore, the magnetic of particulate can be regulated and controled by applying electric field Property, its ferroelectricity can also be regulated and controled；On the other hand, magnetic field is applied to multiferroic liquid, can not only regulates and controls the magnetic of particulate, also Its ferroelectricity can be regulated and controled.Liquid as explanation has magneto-electric coupled performance.More regulation and control can be carried out to multiferroic liquid. There is certain application value in sensor, air locking etc..
Fig. 3 is the TEM figures of CFO-BFO core shell structures, and Fig. 4 is the magnetization curve of CFO-BFO core shell structure particulates, from Fig. 4 In understand, for nano particle, its remanent magnetization is about 20emu/g, coercive field about 300Oe, nano particle magnetic It is stronger.Fig. 5 is the magnetization curve for the CFO-BFO core shell structure multiferroic liquid that volume fraction is 2%, as can be known from Fig. 5, is received Superparamagnetism is presented in rice grain (without remanent magnetism and coercive field).As long as the magnetic field for illustrating to have very little can just make the magnetic of nano particle Square direction changes.

Claims (10)

  1. A kind of 1. multiferroic liquid, it is characterised in that：Nano particle, base fluid and surfactant including multiferroic；It is described to receive The inside of rice grain is magnetic material, and the outer surface of the magnetic material is fully wrapped around by ferroelectric material；The base fluid and described Surfactant is uniformly mixed into mixing liquid, and the nano particle, which is dispersed in, forms stable hang in the mixing liquid Supernatant liquid.
  2. 2. multiferroic liquid according to claim 1, it is characterised in that：Li Jing≤20nm of the nano particle.
  3. 3. multiferroic liquid according to claim 1, it is characterised in that：The nano particle is the nanometer with multiferroic Particulate or nano wire.
  4. 4. multiferroic liquid according to claim 1, it is characterised in that：The base fluid is water, organic liquid or organic water Solution.
  5. 5. multiferroic liquid according to claim 1, it is characterised in that：The base fluid is silicone oil, detergent alkylate or poly- Butylene oil.
  6. 6. multiferroic liquid according to claim 1, it is characterised in that：The surfactant is oleic acid, amino 12 Alkane, fluorine ether acid, laurate, phenyl undecanoic acid are at least one.
  7. 7. prepare the method for any described multiferroic liquid of claim 1 to 5, it is characterised in that：Comprise the following steps：
    Prepare base fluid, surfactant and the nano particle of drying；
    Base fluid and surfactant are uniformly mixed into mixing liquid, then nano particle is added the container equipped with mixing liquid In, shake container and avoid reuniting, precipitate by nano particle is scattered, sealing container is simultaneously placed on to shake on shaking table and makes receiving for multiferroic Rice grain is uniformly dispersed in mixing liquid, so as to the multiferroic liquid that the nano particle volume fraction stablized is V%,
  8. 8. the method according to claim 7 for preparing multiferroic liquid, it is characterised in that：It is small more than half that shaking table shakes the time When.
  9. 9. the method according to claim 7 for preparing multiferroic liquid, it is characterised in that：The V% is less than 20%.
  10. 10. the method according to claim 7 for preparing multiferroic liquid, it is characterised in that：The V% is less than 2%.
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