CN108374209A - Three function Janus nanofiber array films of anisotropic conductive magneto-optic - Google Patents
Three function Janus nanofiber array films of anisotropic conductive magneto-optic Download PDFInfo
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- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
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- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
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- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F10/00—Thin magnetic films, e.g. of one-domain structure
- H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
- H01F10/10—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
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Abstract
The present invention relates to three function Janus nanofiber array films of anisotropic conductive magneto-optic and preparation method thereof, belong to technical field of nanometer material preparation.The present invention includes four steps:(1) precipitation method prepare the Fe of Coated with Oleic Acid3O4It is nanocrystalline;(2) precipitation method prepare Tb (BA)3Phen and Eu (BA)3phen;(3) spinning solution is prepared;(4) three function { [Fe of anisotropic conductive magneto-optic is prepared3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure Janus nanofiber array films, using two strands of special parallel spinning nozzles, aluminum rotating cylinder is reception device, is prepared using electrostatic spinning technique.Prepared Janus nanofiber arrays film has the function of good anisotropic conductive magnetism luminous three simultaneously.The method of the present invention is simple and practicable, can produce in batches.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, in particular relate to three function Janus of anisotropic conductive magneto-optic
Nanofiber array film and preparation method thereof.
Background technology
Anisotropic conductive film is a kind of novel electronic component interconnecting material, it have one direction on electric conductivity and
Insulating properties on other directions, be widely used in Electronic Packaging, chip is fixed and electrode bonding etc. fields, cause
The great attention of people.
Simple function applications to nanostructures is limited in scope, and difunctional or multi-functional nanometer material application range is more
Extensively, this kind of material has more characteristic and attraction, and therefore, multi-functional nanometer material is paid high attention to by researcher.With nanometer
The development of science and technology, nano material such as have the characteristics of luminescence, electric conductivity or magnetism, towards difunctional and more work(by simple function
Can direction develop, such as have the function of magneto-optic, photoelectricity or electromagnetism be difunctional and photoelectromagnetic three, in this way can be in a kind of nanostructure
Difunctional or three functions are realized on material, are had to the development of nano-device, nanotechnology and relevant science and technology important
Meaning.For example, magnetism-fluorescent dual-function nanocomposite provides a kind of new platform for medical diagnosis on disease and treatment, due to
Their difunctional property makes " it was found that-detection-treatment " of disease to be integrally formed.The use of this nanocomposite will be into one
Step improves the efficiency of diagnosis and reduces side effect, causes the highest attention of researcher.Electromagnetism dual-functional nanometer compound is in thunder
It has broad application prospects up to wave absorption, electromagnetic shielding, antistatic coating and sensor etc..
Janus materials refer to two kinds of chemical compositions or a kind of chemical composition but structure difference has clearly in same system
Partitioned organization, thus there is double properties such as hydrophilic/hydrophobic, polar/non-polar, shine/conductive, horizontal direction is conductive/vertical
Direction conduction etc. is one of forward position, hot research direction of materials science field.The Janus nanofibers of document report at present
All be made of shoulder to shoulder and together the different nanofiber of two chemical compositions, tool there are two specific partitioned organization and
Two or more property, as the side nanofiber of Janus nanofibers has lighting function, other side nanofiber
With conductive and magnetic function, then this Janus nanofibers have the function of to shine, are conductive and magnetic three.
Ferroso-ferric oxide Fe3O4It is a kind of important and widely applied magnetic material.People have used a variety of methods, such as
The methods of the precipitation method, sol-gel method, microemulsion method, hydro-thermal and solvent-thermal method, thermal decomposition method, method of electrostatic spinning are successfully made
It is standby gone out Fe3O4The nano materials such as nanocrystalline, nanometer rods, nano wire, nanometer film, hybrid structure, Core-shell Structure Nanoparticles, skill
Art comparative maturity.Rare earth metal terbium coordination compound Tb (BA)3Phen, Tb3+For terbium ion, BA is benzoic acid, and phen is phenanthroline,
Become because of the unique electron configuration of terbium ion it is unique can green luminescent material, as luminous intensity is high, stability is good,
The advantages that fluorescence quantum yield is high, monochromaticjty is good, is a kind of widely applied green fluorescent material.Rare earth metal europium complex Eu
(BA)3Phen, Eu3+For europium ion, BA is benzoic acid, and phen is phenanthroline, is become because of the unique electron configuration of europium ion
The red illuminating material of unique energy, such as luminous intensity is high, stability is good, fluorescence quantum yield is high, monochromaticjty is good excellent
Point is a kind of widely applied red fluorescence material.By Tb (BA)3Phen and Eu (BA)3Phen is mixed according to a certain percentage, can
To obtain different fluorescence colors, the adjustability of fluorescence color is realized.Polyaniline PANI since it is readily synthesized, conductivity is high and
The advantages that environmental stability is good has become one of the hot spot of conducting polymer area research.People synthesized nano wire,
The polyaniline PANI of the one-dimensional nano structures such as nanometer rods, nanotube and nanofiber.Polyvinylpyrrolidone PVP is a kind of honest and clean
Valence, environmental protection and the good common high-molecular matrix material of spinning properties.Therefore, magnetic Fe is utilized3O4It is nanocrystalline, rare earth luminous
Complex Tb (BA)3phen、Eu(BA)3Phen, electrically conductive polyaniline PANI and matrix PVP construct three work(of anisotropic conductive magneto-optic
Energy thin-film material is ideal substance.
Existing research is it has been proved that work as dark colour electrically conductive polyaniline PANI and magnetic Fe3O4It is direct with rare earth compounding
Mixing, can significantly reduce its illumination effect, therefore to obtain the good illumination effect of rare earth compounding, it is necessary to make rare earth compounding
With PANI and Fe3O4Realization efficiently separates.If by electrically conductive polyaniline PANI, magnetic Fe3O4Exist with rare earth compounding difference confinement
In oneself independent space, efficiently separating for three can be thus realized on microcosmic, in macroscopically three function of photoelectromagnetic
It can be highly integrateable on one-dimensional nano structure material again, this novel one-dimensional nano structure material will be with important application
Foreground.In order to realize this academic thought, we design and have constructed [coaxial nano cable] // [nanofiber] special construction
Janus nanofibers.With Fe3O4/ PVP is sandwich layer, with Tb (BA)3phen/Eu(BA)3Phen/PVP is shell, is constituted coaxial
Nano-cable, and PANI/PVP nanofibers and is assembled into { [Fe together3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } the three function Janus nanofibers of photoelectromagnetic of // [PANI/PVP] special construction.With the tool of current document report
The Janus nanofiber differences constituted there are two clear subregion, by [nanofiber] // [nanofiber], what is constructed is [coaxial
Nano-cable] // [nanofiber] special construction Janus nanofibers, tool is there are three specific partitioned organization.Using this
The Janus nanofibers of special construction realize polyaniline PANI, Fe3O4With efficiently separating for rare earth compounding three, to obtain
Obtain-conductive-magnetism three-function nano the fiber of good performance that shines.The Janus nanofibers of this special construction are recycled to make
For construction unit and conductive unit, array films are prepared into, this array films there will be anisotropic conductive, while also assign it
Magneto-optic functional characteristic realizes the multifunction of anisotropic conductive film.This novel nano structural material will be with important
Application prospect has not yet to see relevant document report.
One related electrospinning process (electrospinning) of the U.S. Patent Publication of Patent No. 1975504
Technical solution, this method is to prepare a kind of effective ways of continuous micro nanometer fiber with macro length, by
Formhals was proposed first in 1934.This method is mainly used to prepare high polymer nanometer fiber, it is characterized in that making electrification
Polymer Solution or melt are sprayed by the traction of electrostatic force by nozzle in electrostatic field, invest the receiving screen on opposite, to real
Existing wire drawing, then, evaporation of the solvent or melt are cooled to room temperature and cure at normal temperatures, obtain micro nanometer fiber, these fibers
It is stacked into and is formed micro nanometer fiber film together.People have used uniaxial electrospinning technology to be prepared for the single work(of photoelectromagnetic
Energy, difunctional and three-function nano tunica fibrosa.Q.Z.Yu, et al. are prepared for having single conductive work(using electrostatic spinning technique
The polyaniline PANI nano fibrous membranes [Mater.Sci.Eng.B, 2008,150,70-76] of energy;Dong Xiangting etc. uses electrostatic spinning
Technology is prepared for the PAN/Eu (BA) with single lighting function3Phen luminous nano fibres [New Chemical Materials, 2008,36
(9),49-52];Wang Ce etc. is prepared for having magnetic polyvinylpyrrolidone/ferroso-ferric oxide compound using method of electrostatic spinning
Nanofiber [Chemical Journal of Chinese Universities, 2006,27 (10), 2002-2004];Qingbiao Yang, et al. use electrostatic
Spining technology is prepared for Fe2O3nanoparticles/Eu(DBM)3(Bath) compound difunctional magneto-optic nanofiber [Journal
Of Colloid and Interface Science, 2010,350,396-401], Dong Xiangting etc. uses electrostatic spinning technique system
For Fe3O4/Eu(BA)3Phen/PVP magneto-optic double-functions composite nano fiber [Journal of Nanoparticle
Research,2012,14(10):1203-1209]、Eu(BA)3The difunctional composite nano fiber of phen/PANI/PVP photoelectricity is [high
Equal schools chemistry journal, 2012,33 (8), 1657-1662] and Eu (BA)3phen/PANI/Fe3O4Three function of/PVP photoelectromagnetics is received
Rice fiber [Journal of Materials Science:Materials in Electronics,2014,25(3),1309-
1316].Dong Xiangting etc. uses two strands of parallel spinning nozzles, and [nanofiber] // [nanometer is prepared for using electrostatic spinning technique
Fiber] type magneto-optic double-function Janus nanofibers [Chemical Engineering Journal, 2014,254,259-
267], magnetic photochromic adjustable Janus nanofibers [RSC Advances, 2015,5,35948-35957] and three work(of photoelectromagnetic
It can Janus nanofibers [ChemPlusChem, 2014,79 (5), 690-697].Liu Tianxi of Fudan University etc. is using uniaxial quiet
Electrospinning is prepared for the anisotropic conductive film [Nanoscale, 2015,7,1037-1046] being made of nanofiber.Dong
Phase court of a feudal ruler etc. use two strands of parallel spinning nozzles, using electrostatic spinning technique be prepared for [nanobelt] // [nanobelt] type it is each to
Anisotropic conduction magneto-optic three function Janus nano-band arrays film [national inventing patent, grant number:ZL201410795673.0].Mesh
Before, have no using electrostatic spinning technique prepare [coaxial nano cable] // [nanofiber] special construction Janus nanofibers and
By the relevant report for the anisotropic conductive array films that this special construction Janus nanofibers are constructed.
When preparing nano material using electrostatic spinning technique, the type of raw material, the molecular weight of high polymer templates, spinning solution
Composition, spinning process parameter and spinning head structure the morphology and size of final products is all had a major impact.The present invention makes
The two strands of parallel spinning nozzles constituted with special designing and [coaxial spinning head] // [the uniaxial spinning head] made, using electrostatic
Spining technology, by the Fe of Coated with Oleic Acid3O4Nanocrystalline and polyvinylpyrrolidone PVP be added to N,N-dimethylformamide DMF and
In the mixed solution of chloroform, it is configured to an electrostatic spinning liquid with certain viscosity, referred to as spinning solution I has magnetic function, uses
In the sandwich layer for preparing coaxial nano cable, by Tb (BA)3(phen)、Eu(BA)3(phen) and PVP is added to the mixed of DMF and chloroform
It closes in solution, is configured to the electrostatic spinning liquid with certain viscosity, referred to as spinning solution II, there is lighting function, be used to prepare same
Aniline, camphorsulfonic acid, PVP, DMF, chloroform and ammonium persulfate are mixed and constitute another spinning solution by the shell of axis nano-cable,
Wherein aniline polymerization has conducting function, the nanometer being used to prepare in Janus structures at polyaniline PANI, referred to as spinning solution III
Fiber, the viscosity for controlling spinning solution is most important, using aluminum rotating cylinder as the reception device of Janus nanofibers, best
Process conditions under obtained three function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/
PVP] } // [PANI/PVP] structure Janus nanofiber array films.
Invention content
Photoelectromagnetic simple function is prepared for using uniaxial electrospinning technology in the background technology, difunctional and three functions are received
Rice fiber and anisotropic conductive film, be prepared for using two strands of parallel spinning heads, using electrostatic spinning technique [nanofiber] //
The three function Janus nanofibers of magneto-optic double-function and photoelectromagnetic of [nanofiber] type, and it is prepared for [nanobelt] // [nanometer
Band] type three function Janus nano-band array films of anisotropic conductive magneto-optic.Used raw material, template, solvent and final
Target product and the present invention method it is different.The present invention is using special designing and the two bursts of parallel spinning spinnerets made
Head, aluminum rotating cylinder are prepared for [coaxial nano cable] // [nanofiber] type as reception device using electrostatic spinning technique
{[Fe3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } the Janus Nanowires of // [PANI/PVP] special construction
Dimension, then by this special construction Janus nanofibers as constructing and conductive unit, be prepared for anisotropic conductive magneto-optic three
Function Janus nanofiber array films increase a kind of nanocomposite with novel structure for nano fibrous membrane field.
The invention is realized in this way preparing Tb (BA) using the precipitation method first3phen、Eu(BA)3Phen complexs and
The Fe of Coated with Oleic Acid3O4It is nanocrystalline, by the Fe of Coated with Oleic Acid3O4Nanocrystalline and polyvinylpyrrolidone PVP is added to N, N- diformazans
In the mixed solution of base formamide DMF and chloroform, it is configured to an electrostatic spinning liquid with certain viscosity, referred to as spinning solution I,
With magnetic function, it is used to prepare the sandwich layer of coaxial nano cable, by Tb (BA)3(phen)、Eu(BA)3(phen) it is added to PVP
In the mixed solution of DMF and chloroform, it is configured to the electrostatic spinning liquid with certain viscosity, referred to as spinning solution II, there is the work(that shines
Can, it is used to prepare the shell of coaxial nano cable, aniline, camphorsulfonic acid, PVP, DMF, chloroform and ammonium persulfate are mixed and constituted
Another spinning solution, wherein aniline polymerization have conducting function, are used to prepare at polyaniline PANI, referred to as spinning solution III
Nanofiber in Janus structures, the viscosity for controlling spinning solution are most important.Turned using two strands of parallel spinning nozzles, aluminum
Cylinder carries out electrostatic spinning as reception device and electrostatic spinning technique, under best process conditions, obtains anisotropic conductive
Three function { [Fe of magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } Janus nanometers of // [PANI/PVP] structure
Fiber array film, step are:
(1) precipitation method prepare the Fe of Coated with Oleic Acid3O4It is nanocrystalline
By 5.4060g FeCl3·6H2O, 2.7800g FeSO4·7H2O, 4.04g NH4NO3It is with 1.9000g molecular weight
20000 polyethylene glycol is dissolved in 100mL deionized waters, is heated to 50 DEG C and is passed through argon gas 30min, ammonium hydroxide is then slowly added dropwise
PH value to solution is 11, continues logical argon gas 20min and obtains black suspension, after this suspension Magneto separate, uses absolute ethyl alcohol
It is washed successively with deionized water three times, product is placed in 60 DEG C of vacuum drying chamber dry 12h, obtains a diameter of 8-10nm's
Fe3O4It is nanocrystalline;Take the Fe prepared by 1.5000g3O4It is nanocrystalline to be dispersed in the 100mL deionized waters for being passed through 30min argon gas
And ultrasonic disperse 20min, then solution is heated to 80 DEG C under protection of argon gas, and 1mL oleic acid is added, then proceedes to react
Obtained precipitation is carried out Magneto separate by 40min, is removed water layer and will be deposited in 60 DEG C of vacuum drying chambers dry 6h, obtains
The Fe of Coated with Oleic Acid3O4It is nanocrystalline;
(2) precipitation method prepare Tb (BA)3Phen and Eu (BA)3Phen complexs
By 1.8693g Tb4O7Powder is dissolved in 10mL concentrated nitric acids, and heating is evaporated the extra nitric acid of removing and obtains Tb
(NO3)3·6H2O crystal is added 20mL absolute ethyl alcohols, is configured to Tb (NO3)3Ethanol solution, by 1.8320g benzoic acid and
0.9910g Phens are dissolved in the absolute ethyl alcohol of 100mL jointly, then by prepared Tb (NO3)3Ethanol solution is slowly added to
Wherein, the pH value of solution is adjusted between 6.0-6.5, is heated to 50-60 DEG C, 3h is stirred, by obtained precipitation water and nothing
Water-ethanol washs 3 times successively, and product is placed in 60 DEG C of baking ovens dry 12h, obtains Tb (BA)3Phen powder;By 1.7600g
Eu2O3Powder is dissolved in 10mL concentrated nitric acids, and heating is evaporated the extra nitric acid of removing and obtains Eu (NO3)3·6H2O crystal is added
20mL absolute ethyl alcohols are configured to Eu (NO3)3Ethanol solution, 3.6640g benzoic acid and 1.8020g Phens are dissolved in jointly
In the absolute ethyl alcohol of 100mL, then by prepared Eu (NO3)3Ethanol solution is slowly added thereto, and the pH value for adjusting solution is
Between 6.0-6.5,60 DEG C are heated to, 3h is stirred, obtained precipitation water and absolute ethyl alcohol is washed 3 times successively, by product
It is placed in 60 DEG C of baking ovens dry 12h, obtains Eu (BA)3Phen powder;
(3) spinning solution is prepared
By the Fe of 0.8g Coated with Oleic Acid3O4It is nanocrystalline to be added to 1.6g N,N-dimethylformamide DMF and 6.0696g chloroforms
In mixed liquor and ultrasound 20min, the polyvinylpyrrolidone PVP that 0.8g molecular weight is 1300000 is added, after stirring for 24 hours, is obtained
To spinning solution I;By 0.0563g Tb (BA)3phen、0.0563g Eu(BA)3Phen and 0.75g PVP are added to 5.8259g chlorine
Imitative and 1.5066g DMF in the mixed solvent simultaneously stirs for 24 hours, obtains spinning solution II;0.6g PVP are added to 2.5000g chloroforms
With the in the mixed solvent of 6.5000g DMF and stir 2h, obtain uniform colloidal fluid, add 0.9800g aniline ANI and
1.2220g camphorsulfonic acids CSA and after stirring 2h, is added 0.4411g ammonium persulfates APS and simultaneously stirs 30min, then mixed solution is existed
It in ice-water bath after magnetic agitation 2-3h, is put into 5 DEG C of cold compartment of refrigerator for 24 hours, obtains spinning solution III;
(4) three function { [Fe of anisotropic conductive magneto-optic is prepared3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/
PVP] } // [PANI/PVP] structure Janus nanofiber array films
Two strands of parallel spinning nozzles are made of parallel an individual stainless steel syringe needle and one group of coaxial stainless steel syringe needle,
Truncated 8# stainless steel syringe needles are inserted into truncated 16# stainless steel syringe needles, tip is in same plane and forms coaxial configuration
Syringe needle, after another truncated 12# stainless steel syringe needles are bent 30 °, are fixed to one side of coaxial stainless steel syringe needle, make this root
The tip of stainless steel syringe needle and coaxial stainless steel syringe needle is closely parallel, and is in same plane, finally a 1mL plastics is used to spray
Pipette tips are sleeved on three stainless steel syringe needles, so that the tip of three stainless steel syringe needles is in the middle section of plastic spray gun head, by 8#
The upper 2.5mL syringes of stainless steel syringe needle connection are as interior spin duct, and the upper 5mL syringes of 16# stainless steel syringe needles connection are as outer spinning
Then spinning solution I is added to interior spin duct by fiber tube, the upper 5mL syringes of 12# stainless steel syringe needles connection as individual spin duct
In, spinning solution II is added in outer spin duct, and spinning solution III is added in individual spin duct, using perpendicular spray mode, receives dress
It is set to the aluminum rotating cylinder of long 20cm, a diameter of 8cm, other spinning parameters are:Spinning voltage is 10kV, and needle point is with rotating cylinder spacing
13cm, environment temperature are 22-25 DEG C, relative humidity 20%-30%, and rotating cylinder rotating speed is 1500rmin-1, obtain anisotropy and lead
Three function { [Fe of electromagnetism light3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure Janus receives
Rice fiber array film.
Prepared three function Janus nanofiber array films of anisotropic conductive magneto-optic in above process, by
{[Fe3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure Janus nanofibers are according to one
A direction arranges, { [Fe3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure
Janus nanofibers by coaxial nano cable and nanofiber shoulder to shoulder and together with form, coaxial nano cable and nanometer
The average diameter of fiber is 600nm;Under the ultraviolet excitation of 276nm, three function Janus Nanowires of anisotropic conductive magneto-optic
Dimension array films launch yellow-green fluorescence;The saturated magnetization of three function Janus nanofiber array films of anisotropic conductive magneto-optic
Intensity is 4.98emug-1;Along on Janus nanofiber lengths direction, Janus nanometers of three function of anisotropic conductive magneto-optic
The conductivity of fiber array film is 1.86Scm-1, and on Janus nanofiber lengths direction, anisotropic conductive
The conductivity of three function Janus nanofiber array films of magneto-optic is 6.27 × 10-7S·cm-1, the two ratio is 2.97 × 106, tool
There is a good anisotropic conductive characteristic, prepared three function Janus nanofiber array films of anisotropic conductive magneto-optic, together
When have the function of good anisotropic conductive, magnetism and shine three, realize goal of the invention.
Description of the drawings
Fig. 1 is three function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/
PVP] } XRD spectras of // [PANI/PVP] structure Janus nanofiber array films;
Fig. 2 is three function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/
PVP] } the TEM photos of // [PANI/PVP] structure Janus nanofiber array films;
Fig. 3 is three function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/
PVP] } SEM photographs of // [PANI/PVP] structure Janus nanofiber array films, which also serves as Figure of abstract;
Fig. 4 is to monitor three function { [Fe of anisotropic conductive magneto-optic when wavelength is 545nm3O4/PVP]@[Tb(BA)3phen/
Eu(BA)3Phen/PVP] } exciting light spectrograms of // [PANI/PVP] structure Janus nanofiber array films;
Fig. 5 is to monitor three function { [Fe of anisotropic conductive magneto-optic when wavelength is 616nm3O4/PVP]@[Tb(BA)3phen/
Eu(BA)3Phen/PVP] } exciting light spectrograms of // [PANI/PVP] structure Janus nanofiber array films;
Fig. 6 is three function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/
PVP] } launching light spectrograms of // [PANI/PVP] structure Janus nanofiber array films;
Fig. 7 is three function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/
PVP] } the CIE chromaticity coordinates figures of // [PANI/PVP] structure Janus nanofiber array films;
Fig. 8 is three function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/
PVP] } the hysteresis loop figures of // [PANI/PVP] structure Janus nanofiber array films.
Specific implementation mode
Terbium oxide Tb selected by the present invention4O7With europium oxide Eu2O3Purity be 99.99%, benzoic acid, Phen,
N,N-Dimethylformamide, chloroform, Iron(III) chloride hexahydrate, green vitriol, ammonium nitrate, molecular weight be 20000 it is poly-
Ethylene glycol, nitric acid, the polyvinylpyrrolidone that molecular weight is 1300000, absolute ethyl alcohol, ammonium hydroxide, aniline, camphorsulfonic acid, over cure
Sour ammonium, oleic acid, argon gas are commercially available analysis net product;It makes by oneself in deionized water laboratory;Glass apparatus and equipment used is real
Test common instrument and equipment in room.
Embodiment:By 5.4060g FeCl3·6H2O, 2.7800g FeSO4·7H2O, 4.04g NH4NO3And 1.9000g
The polyethylene glycol that molecular weight is 20000 is dissolved in 100mL deionized waters, is heated to 50 DEG C and is passed through argon gas 30min, then slowly
The pH value that ammonium hydroxide is added dropwise to solution is 11, continues logical argon gas 20min and obtains black suspension, after this suspension Magneto separate, uses
Absolute ethyl alcohol and deionized water are washed three times successively, and product is placed in 60 DEG C of vacuum drying chamber dry 12h, is obtained a diameter of
The Fe of 8-10nm3O4It is nanocrystalline;Take the Fe prepared by 1.5000g3O4Nanocrystalline be dispersed in has been passed through the 100mL of 30min argon gas
In ionized water and ultrasonic disperse 20min, then solution is heated to 80 DEG C under protection of argon gas, and 1mL oleic acid is added, then after
Continuous reaction 40min, Magneto separate is carried out by obtained precipitation, is removed water layer and will be deposited in 60 DEG C of vacuum drying chambers dry
6h obtains the Fe of Coated with Oleic Acid3O4It is nanocrystalline;By 1.8693g Tb4O7Powder is dissolved in 10mL concentrated nitric acids, and heating, which is evaporated, to remove
Extra nitric acid is gone to obtain Tb (NO3)3·6H2O crystal is added 20mL absolute ethyl alcohols, is configured to Tb (NO3)3Ethanol solution, will
1.8320g benzoic acid and 0.9910g Phens are dissolved in the absolute ethyl alcohol of 100mL jointly, then by prepared Tb (NO3)3Second
Alcoholic solution is slowly added thereto, and adjusts the pH value of solution between 6.0-6.5, is heated to 50-60 DEG C, stirs 3h, will be acquired
Precipitation water and absolute ethyl alcohol wash successively 3 times, product is placed in 60 DEG C of baking ovens dry 12h, obtains Tb (BA)3Phen powder
End;By 1.7600g Eu2O3Powder is dissolved in 10mL concentrated nitric acids, and heating is evaporated the extra nitric acid of removing and obtains Eu (NO3)3·
6H2O crystal is added 20mL absolute ethyl alcohols, is configured to Eu (NO3)3Ethanol solution, 3.6640g benzoic acid and 1.8020g is adjacent
Phenanthroline is dissolved in the absolute ethyl alcohol of 100mL jointly, then by prepared Eu (NO3)3Ethanol solution is slowly added thereto, and is adjusted
The pH value of solution is heated to 60 DEG C between 6.0-6.5, stirs 3h, obtained precipitation water and absolute ethyl alcohol are washed successively
It washs 3 times, product is placed in 60 DEG C of baking ovens dry 12h, obtains Eu (BA)3Phen powder;By the Fe of 0.8g Coated with Oleic Acid3O4It receives
Meter Jing is added in 1.6g n,N-Dimethylformamide DMF and 6.0696g chloroform mixed liquors and ultrasound 20min, adds 0.8g
The polyvinylpyrrolidone PVP that molecular weight is 1300000 obtains spinning solution I after stirring for 24 hours;By 0.0563g Tb (BA)3phen、0.0563g Eu(BA)3Phen and 0.75g PVP are added to the in the mixed solvent of 5.8259g chloroforms and 1.5066g DMF
And stir for 24 hours, obtain spinning solution II;0.6g PVP are added to the in the mixed solvent of 2.5000g chloroforms and 6.5000g DMF simultaneously
2h is stirred, uniform colloidal fluid is obtained, after adding 0.9800g aniline ANI and 1.2220g camphorsulfonic acid CSA and stirring 2h, adds
Enter 0.4411g ammonium persulfates APS and stir 30min, then mixed solution after magnetic agitation 2-3h, is put into 5 DEG C in ice-water bath
Cold compartment of refrigerator in for 24 hours, obtain spinning solution III;Two strands of parallel spinning nozzles are by an individual stainless steel syringe needle and one
The coaxial stainless steel syringe needle of group is constituted parallel, truncated 8# stainless steel syringe needles is inserted into truncated 16# stainless steel syringe needles, tip
The syringe needle that coaxial configuration is formed in same plane after another truncated 12# stainless steel syringe needle is bent 30 °, is fixed to same
One side of axis stainless steel syringe needle keeps the tip of this root stainless steel syringe needle and coaxial stainless steel syringe needle closely parallel, and in same
Plane finally uses a 1mL plastic spray guns headgear on three stainless steel syringe needles, the tip of three stainless steel syringe needles is made to be in
8# stainless steel syringe needles are connected upper 2.5mL syringes as interior spin duct, 16# stainless pins by the middle section of plastic spray gun head
The upper 5mL syringes of head connection are as outer spin duct, and the upper 5mL syringes of 12# stainless steel syringe needles connection are as individual spin duct, so
Spinning solution I is added in interior spin duct afterwards, spinning solution II is added in outer spin duct, and spinning solution III is added to individual spinning
In fiber tube, using perpendicular spray mode, reception device is the aluminum rotating cylinder of long 20cm, a diameter of 8cm, and other spinning parameters are:Spinning
Voltage is 10kV, and needle point is 13cm with rotating cylinder spacing, and environment temperature is 22-25 DEG C, relative humidity 20%-30%, rotating cylinder rotating speed
For 1500rmin-1, obtain three function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/
PVP] } // [PANI/PVP] structure Janus nanofiber array films.Three the function { [Fe of anisotropic conductive magneto-optic3O4/
PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } in // [PANI/PVP] structure Janus nanofiber array films containing vertical
Square phase Fe3O4It is nanocrystalline, as shown in Figure 1;Three the function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } Janus nanofibers in // [PANI/PVP] structure Janus nanofiber array films, be
It is made of shoulder to shoulder and together a coaxial nano cable and a nanofiber, forms Janus structures, co-axial nano electricity
The sandwich layer of cable is Fe3O4/ PVP, shell are Tb (BA)3phen/Eu(BA)3Phen/PVP, nanofiber are PANI/PVP, see Fig. 2
It is shown;Three the function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/PVP]}//
In [PANI/PVP] structure Janus nanofiber array films, Janus nanofibers are arranged according to a direction, and composition Janus receives
The coaxial nano cable of rice fiber and the average diameter of nanofiber are 600nm, as shown in Figure 3;Using 545nm as monitoring wave
It is long, three function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/PVP]}//[PANI/
PVP] there are one wide excitation bands, peak value can return at 276nm at 200-360nm for structure Janus nanofiber array films
For π → π * transition of ligand, as shown in Figure 4;Using 616nm as monitoring wavelength, three function { [Fe of anisotropic conductive magneto-optic3O4/
PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure Janus nanofiber array films are in 200-
There are one wide excitation bands, peak value can be classified as π → π * transition of ligand, as shown in Figure 5 at 276nm at 355nm;
Under the ultraviolet excitation of 276nm, three function { [Fe of anisotropic conductive magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure Janus nanofiber array films launch main peak and are located at 490nm, 545nm,
At 592nm, 616nm, it corresponds to Tb3+'s5D4→7F6(490nm)、5D4→7F5(545nm) and Eu3+'s5D0→7F1
(592nm)、5D0→7F2(616nm) energy level transition, as shown in Figure 6;Under the ultraviolet excitation of 276nm, anisotropic conductive magnetic
Three function { [Fe of light3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure Janus Nanowires
Dimension array films launch yellow-green fluorescence, and chromaticity coordinates x, y are respectively 0.336,0.558, as shown in Figure 7;It is made state it is each to different
Three function { [Fe of property conduction magneto-optic3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure
Janus nanofiber array films have stronger magnetism, saturation magnetization 4.98emug-1, as shown in Figure 8;Using suddenly
Your effect tester is measured along on Janus nanofiber lengths direction, three function Janus Nanowires of anisotropic conductive magneto-optic
The conductivity for tieing up array films is 1.86Scm-1, and on Janus nanofiber lengths direction, anisotropic conductive magnetic
The conductivity of three function Janus nanofiber array films of light is 6.27 × 10-7S·cm-1, the two ratio is 2.97 × 106, have
Good anisotropic conductive characteristic.
Certainly, the invention may also have other embodiments, without deviating from the spirit and substance of the present invention, ripe
It knows those skilled in the art and makes various corresponding change and deformations, but these corresponding changes and change in accordance with the present invention
Shape should all belong to the protection domain of appended claims of the invention.
Claims (2)
1. three function Janus nanofiber array films of anisotropic conductive magneto-optic, which is characterized in that by { [Fe3O4/PVP]@[Tb
(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure Janus nanofibers arrange according to a direction,
{[Fe3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure Janus nanofibers are by coaxial
Nano-cable and nanofiber shoulder to shoulder and together with form, the average diameter of coaxial nano cable and nanofiber is
600nm, three function Janus nanofiber arrays film of anisotropic conductive magneto-optic have good anisotropic conductive, magnetic simultaneously
Property and shine three functions.
2. a kind of preparation side of three function Janus nanofiber array films of anisotropic conductive magneto-optic as described in claim 1
Method, which is characterized in that using special designing and the two strands of parallel spinning nozzles made, aluminum rotating cylinder is as reception device, profit
With electrostatic spinning technique, it is three function { [Fe of anisotropic conductive magneto-optic to prepare product3O4/PVP]@[Tb(BA)3phen/Eu
(BA)3Phen/PVP] } // [PANI/PVP] structure Janus nanofiber array films, step is:
(1) precipitation method prepare the Fe of Coated with Oleic Acid3O4It is nanocrystalline
By 5.4060g FeCl3·6H2O, 2.7800g FeSO4·7H2O, 4.04g NH4NO3It is with 1.9000g molecular weight
20000 polyethylene glycol is dissolved in 100mL deionized waters, is heated to 50 DEG C and is passed through argon gas 30min, ammonium hydroxide is then slowly added dropwise
PH value to solution is 11, continues logical argon gas 20min and obtains black suspension, after this suspension Magneto separate, uses absolute ethyl alcohol
It is washed successively with deionized water three times, product is placed in 60 DEG C of vacuum drying chamber dry 12h, obtains a diameter of 8-10nm's
Fe3O4It is nanocrystalline;Take the Fe prepared by 1.5000g3O4It is nanocrystalline to be dispersed in the 100mL deionized waters for being passed through 30min argon gas
And ultrasonic disperse 20min, then solution is heated to 80 DEG C under protection of argon gas, and 1mL oleic acid is added, then proceedes to react
Obtained precipitation is carried out Magneto separate by 40min, is removed water layer and will be deposited in 60 DEG C of vacuum drying chambers dry 6h, obtains
The Fe of Coated with Oleic Acid3O4It is nanocrystalline;
(2) precipitation method prepare Tb (BA)3Phen and Eu (BA)3Phen complexs
By 1.8693g Tb4O7Powder is dissolved in 10mL concentrated nitric acids, and heating is evaporated the extra nitric acid of removing and obtains Tb (NO3)3·
6H2O crystal is added 20mL absolute ethyl alcohols, is configured to Tb (NO3)3Ethanol solution, 1.8320g benzoic acid and 0.9910g is adjacent
Phenanthroline is dissolved in the absolute ethyl alcohol of 100mL jointly, then by prepared Tb (NO3)3Ethanol solution is slowly added thereto, and is adjusted
The pH value of solution is heated to 50-60 DEG C between 6.0-6.5, stirs 3h, successively by obtained precipitation water and absolute ethyl alcohol
Product is placed in 60 DEG C of baking ovens dry 12h, obtains Tb (BA) by washing 3 times3Phen powder;By 1.7600g Eu2O3Powder is molten
In 10mL concentrated nitric acids, heating is evaporated the extra nitric acid of removing and obtains Eu (NO solution3)3·6H2The anhydrous second of 20mL is added in O crystal
Alcohol is configured to Eu (NO3)3Ethanol solution, 3.6640g benzoic acid and 1.8020g Phens are dissolved in the nothing of 100mL jointly
In water-ethanol, then by prepared Eu (NO3)3Ethanol solution is slowly added thereto, and adjusts the pH value of solution between 6.0-6.5,
60 DEG C are heated to, 3h is stirred, obtained precipitation water and absolute ethyl alcohol is washed 3 times successively, product is placed on 60 DEG C of baking ovens
Middle dry 12h obtains Eu (BA)3Phen powder;
(3) spinning solution is prepared
By the Fe of 0.8g Coated with Oleic Acid3O4It is nanocrystalline to be added to the mixing of 1.6g N,N-dimethylformamide DMF and 6.0696g chloroforms
In liquid and ultrasound 20min, the polyvinylpyrrolidone PVP that 0.8g molecular weight is 1300000 is added, after stirring for 24 hours, is spun
Silk liquid I;By 0.0563g Tb (BA)3phen、0.0563g Eu(BA)3Phen and 0.75g PVP be added to 5.8259g chloroforms and
The in the mixed solvent of 1.5066g DMF simultaneously stirs for 24 hours, obtains spinning solution II;By 0.6g PVP be added to 2.5000g chloroforms and
The in the mixed solvent of 6.5000g DMF simultaneously stirs 2h, obtains uniform colloidal fluid, add 0.9800g aniline ANI and
1.2220g camphorsulfonic acids CSA and after stirring 2h, is added 0.4411g ammonium persulfates APS and simultaneously stirs 30min, then mixed solution is existed
It in ice-water bath after magnetic agitation 2-3h, is put into 5 DEG C of cold compartment of refrigerator for 24 hours, obtains spinning solution III;
(4) three function { [Fe of anisotropic conductive magneto-optic is prepared3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/PVP]}//
[PANI/PVP] structure Janus nanofiber array films
Two strands of parallel spinning nozzles are made of parallel an individual stainless steel syringe needle and one group of coaxial stainless steel syringe needle, will be cut
Flat 8# stainless steel syringe needles are inserted into truncated 16# stainless steel syringe needles, and tip is in the needle that same plane forms coaxial configuration
Head is fixed to one side of coaxial stainless steel syringe needle, keeps this root stainless after another truncated 12# stainless steel syringe needle is bent 30 °
The tip of draw point head and coaxial stainless steel syringe needle is closely parallel, and is in same plane, finally uses a 1mL plastic spray gun head
It is sleeved on three stainless steel syringe needles, the tip of three stainless steel syringe needles is made to be in the middle section of plastic spray gun head, 8# is stainless
The upper 2.5mL syringes of draw point head connection as interior spin duct, the upper 5mL syringes of 16# stainless steel syringe needles connection as outer spin duct,
Then spinning solution I is added in interior spin duct, spins as individual spin duct by the upper 5mL syringes of 12# stainless steel syringe needles connection
Silk liquid II is added in outer spin duct, and spinning solution III is added in individual spin duct, and using perpendicular spray mode, reception device is
The aluminum rotating cylinder of long 20cm, a diameter of 8cm, other spinning parameters are:Spinning voltage is 10kV, and needle point is with rotating cylinder spacing
13cm, environment temperature are 22-25 DEG C, relative humidity 20%-30%, and rotating cylinder rotating speed is 1500rmin-1, obtain anisotropy and lead
Three function { [Fe of electromagnetism light3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure Janus receives
Rice fiber array film, by { [Fe3O4/PVP]@[Tb(BA)3phen/Eu(BA)3Phen/PVP] } // [PANI/PVP] structure
Janus nanofibers are arranged according to a direction, { [Fe3O4/PVP]@[Tb(BA)3phen/Eu(BA)3phen/
PVP] } // [PANI/PVP] structure Janus nanofibers by coaxial nano cable and nanofiber shoulder to shoulder and together with group
At the average diameter of coaxial nano cable and nanofiber is 600nm;Under the ultraviolet excitation of 276nm, anisotropic conductive
Three function Janus nanofiber array films of magneto-optic launch yellow-green fluorescence;Janus nanometers of three function of anisotropic conductive magneto-optic
The saturation magnetization of fiber array film is 4.98emug-1;Along on Janus nanofiber lengths direction, anisotropy is led
The conductivity of three function Janus nanofiber array films of electromagnetism light is 1.86Scm-1, and perpendicular to Janus nano fiber longs
It spends on direction, the conductivity of three function Janus nanofiber array films of anisotropic conductive magneto-optic is 6.27 × 10-7S·cm-1,
The two ratio is 2.97 × 106, there is good anisotropic conductive characteristic, prepared three function of anisotropic conductive magneto-optic
Janus nanofiber array films, while having the function of good anisotropic conductive, magnetism and luminous three.
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