CN108277549A - Three function Janus nanofibers of green fluorescence electromagnetism and preparation method thereof - Google Patents
Three function Janus nanofibers of green fluorescence electromagnetism and preparation method thereof Download PDFInfo
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- CN108277549A CN108277549A CN201810104402.4A CN201810104402A CN108277549A CN 108277549 A CN108277549 A CN 108277549A CN 201810104402 A CN201810104402 A CN 201810104402A CN 108277549 A CN108277549 A CN 108277549A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- 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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- 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
- D01F1/10—Other agents for modifying properties
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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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- D—TEXTILES; PAPER
- 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
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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Abstract
The present invention relates to three function Janus nanofibers of green fluorescence electromagnetism 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;(3) spinning solution is prepared, prepares three kinds of spinning solutions respectively;(4) three function [(Fe of green fluorescence electromagnetism is prepared3O4/PVP)@(Tb(BA)3Phen/PVP)] // [PANI/PVP] Janus nanofibers are prepared using special designing and the two strands of parallel spinning nozzles made using electrostatic spinning technique.Prepared three function Janus nanofibers of green fluorescence electromagnetism have the function of good green emitting electroconductive magnetic three simultaneously.The method of the present invention is simple and practicable, can produce in batches, this novel one-dimensional nano structure material has broad application prospects.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, in particular relate to Janus nanometers of three function of green fluorescence electromagnetism
Fiber and preparation method thereof.
Background technology
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.Polyaniline PANI is held due to it
It is easily-synthesized, the advantages that conductivity is high and environmental stability is good, has become one of the hot spot of conducting polymer area research.People
The polyaniline PANI of the one-dimensional nano structures such as nano wire, nanometer rods, nanotube and nanofiber is synthesized.Polyvinyl pyrrole
Alkanone PVP is a kind of cheap, environmentally friendly and good common high-molecular matrix material of spinning properties.Therefore, magnetic Fe is utilized3O4
Nanocrystalline, rare earth terbium emitting complexes Tb (BA)3Phen, electrically conductive polyaniline PANI and matrix PVP are constructed with three work(of photoelectromagnetic
The one-dimensional nano structure material of energy characteristic 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/PVP is shell, constitutes coaxial nano cable, with
PANI/PVP nanofibers are simultaneously assembled into [(Fe together3O4/PVP)@(Tb(BA)3Phen/PVP)] // [PANI/PVP] green
Three function Janus nanofibers of fluorescent electromagnetic.With the tool of current document report there are two clear subregion, by [nanofiber] //
The Janus nanofibers that [nanofiber] is constituted are different, and what is constructed is that [coaxial nano cable] // [nanofiber] is special
The Janus nanofibers of structure, there are three specific partitioned organizations for tool.It is real using the Janus nanofibers of this special construction
Polyaniline PANI, Fe are showed3O4With efficiently separating for rare earth compounding three, to obtain it is of good performance shine-conduction-magnetic
Property three-function nano fiber.This novel nano structural material will be with important application prospects, 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 fiber.Q.Z.Yu, et al. are prepared for having single conducting function using electrostatic spinning technique
Polyaniline PANI nanofibers [Mater.Sci.Eng.B, 2008,150,70-76];Dong Xiangting etc. uses electrostatic spinning technique
It 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 composite Nano using method of electrostatic spinning
Fiber [Chemical Journal of Chinese Universities, 2006,27 (10), 2002-2004];Qingbiao Yang, et al. use electrostatic spinning
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. is prepared using electrostatic spinning technique
Fe3O4/Eu(BA)3Phen/PVP magneto-optic double-functions composite nano fiber [Journal of Nanoparticle
Research,2012,14(10):1203-1209]、Tb(BA)3The difunctional composite nano fiber of phen/PANI/PVP photoelectricity [is changed
Learn journal, 2012,70 (14), 1576-1582] and Eu (BA)3phen/PANI/Fe3O4/ PVP photoelectromagnetic three-function nano fibers
[Journal of Materials Science:Materials in Electronics,2014,25(3),1309-1316]。
Dong Xiangting etc. uses two strands of parallel spinning nozzles, and [nanofiber] // [nanofiber] type is prepared for using electrostatic spinning technique
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 function Janus of photoelectromagnetic receive
Rice fiber [ChemPlusChem, 2014,79 (5), 690-697].It [is coaxially received currently, having no and being prepared using electrostatic spinning technique
Rice cable] // [nanofiber] special construction Janus nanofibers relevant report.
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) it is added in the mixed solution of DMF and chloroform, prepares with PVP
At the electrostatic spinning liquid with certain viscosity, referred to as spinning solution II, there is lighting function, be used to prepare the shell of coaxial nano cable
Layer, by aniline, camphorsulfonic acid, PVP, DMF, chloroform and ammonium persulfate mix constitute another spinning solution, wherein aniline polymerization at
There is conducting function, the nanofiber being used to prepare in Janus structures to control spinning by polyaniline PANI, referred to as spinning solution III
The viscosity of liquid is most important, and [(Fe has been obtained under best process conditions3O4/PVP)@(Tb(BA)3phen/PVP)]//
Three function Janus nanofibers of [PANI/PVP] green fluorescence electromagnetism.
Invention content
Photoelectromagnetic simple function is prepared for using uniaxial electrospinning technology in the background technology, difunctional and three functions are received
Rice fiber, using two strands of parallel spinning nozzles, is prepared for [nanofiber] // [nanofiber] type using electrostatic spinning technique
Three function Janus nanofibers of magneto-optic double-function and photoelectromagnetic, used raw material, template, solvent and final target
Product and the method for the present invention are different.The present invention is using special designing and the two strands of parallel spinning nozzles made, utilization
Electrostatic spinning technique is prepared for the [(Fe of [coaxial nano cable] // [nanofiber] type3O4/PVP)@(Tb(BA)3phen/
PVP)] // three function Janus nanofibers of [PANI/PVP] green fluorescence electromagnetism, increasing one kind for nanofiber field has
The nanocomposite of novel structure.
The invention is realized in this way preparing Tb (BA) using the precipitation method first3Phen complexs and Coated with Oleic Acid
Fe3O4It is nanocrystalline, by the Fe of Coated with Oleic Acid3O4Nanocrystalline and polyvinylpyrrolidone PVP is added to N,N-dimethylformamide
In the mixed solution of DMF and chloroform, it is configured to an electrostatic spinning liquid with certain viscosity, referred to as spinning solution I has magnetic work(
Can, it is used to prepare the sandwich layer of coaxial nano cable, by Tb (BA)3(phen) and PVP is added to the mixed solution of DMF and chloroform
In, it is configured to the electrostatic spinning liquid with certain viscosity, referred to as spinning solution II, there is lighting function, be used to prepare co-axial nano
Aniline, camphorsulfonic acid, PVP, DMF, chloroform and ammonium persulfate are mixed and constitute another spinning solution, wherein benzene by the shell of cable
Amine aggregates into polyaniline PANI, referred to as spinning solution III, with conducting function, the nanofiber being used to prepare in Janus structures,
The viscosity for controlling spinning solution is most important.Electrostatic spinning is carried out using two strands of parallel spinning nozzles and electrostatic spinning technique,
Under best process conditions, [(Fe is obtained3O4/PVP)@(Tb(BA)3Phen/PVP)] // [PANI/PVP] green fluorescence electromagnetism three
Function Janus nanofibers, 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 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;
(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 0.75g PVP and 0.1125g Tb (BA)3Phen complexs are added to 5.8259g chloroforms and 1.5066g
The in the mixed solvent of DMF simultaneously stirs for 24 hours, obtains spinning solution II;0.6g PVP are added to 1.0125g chloroforms and 6.6282g
The in the mixed solvent of DMF simultaneously stirs 2h, obtains uniform colloidal fluid, adds 0.18g aniline ANI and 0.2245g camphorsulfonic acids
CSA and after stirring 2h, is added 0.4411g ammonium persulfates APS and simultaneously stirs 30min, then magnetic force stirs in ice-water bath by mixed solution
It after mixing 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 green fluorescence electromagnetism is prepared3O4/PVP)@(Tb(BA)3phen/PVP)]//[PANI/PVP]
Janus nanofibers
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 wire netting, other spinning parameters are:Spinning voltage is 13kV, and needle point is 16cm, environment temperature 20- with collecting net spacing
26 DEG C, relative humidity 20%-40%, obtain three function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb(BA)3phen/PVP)]//
[PANI/PVP] Janus nanofibers.
Prepared [(Fe in above process3O4/PVP)@(Tb(BA)3Phen/PVP)] // [PANI/PVP] Janus receives
Rice fiber, by coaxial nano cable and nanofiber shoulder to shoulder and together with form, coaxial nano cable and nanofiber
Average diameter is 600nm;Under the ultraviolet excitation of 276nm, [(Fe3O4/PVP)@(Tb(BA)3phen/PVP)]//[PANI/
PVP] Janus nanofibers launch the bright green light that main peak is located at 545nm;[(Fe3O4/PVP)@(Tb(BA)3phen/
PVP)] // [PANI/PVP] average conductivity of Janus nanofibers is 1.460 × 10-4S·cm-1;[(Fe3O4/PVP)@(Tb
(BA)3Phen/PVP)] // [PANI/PVP] saturation magnetization of Janus nanofibers is 7.30emu/g, prepared spy
Different structure Janus nanofibers have the function of good green emitting-conduction-magnetism three, realize goal of the invention.
Description of the drawings
Fig. 1 is three function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb(BA)3phen/PVP)]//[PANI/PVP]
The XRD spectra of Janus nanofibers;
Fig. 2 is three function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb(BA)3phen/PVP)]//[PANI/PVP]
The TEM photos of Janus nanofibers, the figure also serve as Figure of abstract;
Fig. 3 is three function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb(BA)3phen/PVP)]//[PANI/PVP]
The SEM photograph of Janus nanofibers;
Fig. 4 is three function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb(BA)3phen/PVP)]//[PANI/PVP]
The exciting light spectrogram of Janus nanofibers;
Fig. 5 is three function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb(BA)3phen/PVP)]//[PANI/PVP]
The launching light spectrogram of Janus nanofibers;
Fig. 6 is three function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb(BA)3phen/PVP)]//[PANI/PVP]
The hysteresis loop figure of Janus nanofibers.
Specific implementation mode
Terbium oxide Tb selected by the present invention4O7Purity be 99.99%, benzoic acid, Phen, N, N- dimethyl methyls
Amide, chloroform, Iron(III) chloride hexahydrate, green vitriol, ammonium nitrate, the polyethylene glycol that molecular weight is 20000, nitric acid,
The polyvinylpyrrolidone that molecular weight is 1300000, absolute ethyl alcohol, ammonium hydroxide, aniline, camphorsulfonic acid, ammonium persulfate, oleic acid, argon
Gas is commercially available analysis net product;It makes by oneself in deionized water laboratory;Glass apparatus and equipment used is common in laboratory
Instrument and equipment.
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 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 0.75g PVP and 0.1125g Tb (BA)3Phen complexs are added to 5.8259g chloroforms and 1.5066g DMF's
In the mixed solvent simultaneously stirs for 24 hours, obtains spinning solution II;0.6g PVP are added to the mixed of 1.0125g chloroforms and 6.6282g DMF
In bonding solvent and 2h is stirred, obtains uniform colloidal fluid, add 0.18g aniline ANI and 0.2245g camphorsulfonic acid CSA and is stirred
After mixing 2h, 0.4411g ammonium persulfates APS is added and simultaneously stirs 30min, then by mixed solution in ice-water bath magnetic agitation 2-3h
Afterwards, it is put into 5 DEG C of cold compartment of refrigerator for 24 hours, obtains spinning solution III;Two strands of parallel spinning nozzles are individually stainless by one
Draw point head and one group of coaxial stainless steel syringe needle are constituted parallel, and truncated 8# stainless steel syringe needles are inserted into truncated 16# stainless steels
In syringe needle, tip is in the syringe needle that same plane forms coaxial configuration, and another truncated 12# stainless steel syringe needle is bent 30 °
Afterwards, it is fixed to one side of coaxial stainless steel syringe needle, keeps the tip of this root stainless steel syringe needle and coaxial stainless steel syringe needle closely parallel,
And it is in same plane, it finally uses a 1mL plastic spray guns headgear on three stainless steel syringe needles, makes three stainless steel syringe needles
Tip be in the middle section of plastic spray gun head, 8# stainless steel syringe needles are connected into upper 2.5mL syringes as interior spin duct,
The upper 5mL syringes of 16# stainless steel syringe needles connection are as outer spin duct, and the upper 5mL syringes of 12# stainless steel syringe needles connection are as independent
Spin duct, then spinning solution I is added in interior spin duct, spinning solution II is added in outer spin duct, and spinning solution III is added
Into individual spin duct, using perpendicular spray mode, reception device is wire netting, and other spinning parameters are:Spinning voltage is 13kV,
Needle point and collecting net spacing 16cm, environment temperature are 20-26 DEG C, relative humidity 20%-40%, obtain three work(of green fluorescence electromagnetism
It can [(Fe3O4/PVP)@(Tb(BA)3Phen/PVP)] // [PANI/PVP] Janus nanofibers.The green fluorescence electromagnetism
Three function [(Fe3O4/PVP)@(Tb(BA)3Phen/PVP)] // [PANI/PVP] contain cubic phase Fe in Janus nanofibers3O4
It is nanocrystalline, as shown in Figure 1;Three the function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb(BA)3phen/PVP)]//
[PANI/PVP] Janus nanofibers are made of shoulder to shoulder and together a coaxial nano cable and a nanofiber,
Janus structures are formed, the sandwich layer of coaxial nano cable is Fe3O4/ PVP, shell are Tb (BA)3Phen/PVP, nanofiber are
PANI/PVP, as shown in Figure 2;Three the function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb(BA)3phen/PVP)]//
In [PANI/PVP] Janus nanofibers, the average diameter of coaxial nano cable and nanofiber is 600nm, as shown in Figure 3;
Using 545nm as monitoring wavelength, three function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb(BA)3phen/PVP)]//[PANI/
PVP] there are one wide excitation bands, peak value can be classified as the π of ligand at 276nm at 200-375nm for Janus nanofibers
→ π * transition, as shown in Figure 4;Under the ultraviolet excitation of 276nm, three function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb
(BA)3Phen/PVP)] // [PANI/PVP] Janus nanofibers launch the bright green light that main peak is located at 545nm, it is corresponded to
In Tb3+'s5D4→5F5Energy level transition, as shown in Figure 5;Made three the function [(Fe of green fluorescence electromagnetism stated3O4/PVP)@(Tb
(BA)3Phen/PVP)] // [PANI/PVP] Janus nanofibers have stronger magnetism, saturation magnetization 7.30emu/
G, as shown in Figure 6;Three function [(Fe of green fluorescence electromagnetism is measured using Hall effect tester3O4/PVP)@(Tb(BA)3phen/
PVP)] // [PANI/PVP] average conductivity of Janus nanofibers is 1.460 × 10-4S·cm-1。
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 nanofibers of green fluorescence electromagnetism, which is characterized in that by (Fe3O4/PVP)@(Tb(BA)3phen/
PVP) coaxial nano cable and PANI/PVP nanofibers shoulder to shoulder and together with form Janus nanofibers, have simultaneously
The average diameter of green emitting, conduction and magnetic three kinds of functions, coaxial nano cable and nanofiber is 600nm.
2. a kind of preparation method of three function Janus nanofibers of green fluorescence electromagnetism as described in claim 1, feature exist
In using special designing and the two strands of parallel spinning nozzles made, using electrostatic spinning technique, it is [(Fe to prepare product3O4/
PVP)@(Tb(BA)3Phen/PVP)] // [PANI/PVP] Janus nanofibers, 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 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;
(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 0.75g PVP and 0.1125g Tb (BA)3Phen complexs are added to 5.8259g chloroforms and 1.5066g DMF's
In the mixed solvent simultaneously stirs for 24 hours, obtains spinning solution II;0.6g PVP are added to the mixed of 1.0125g chloroforms and 6.6282g DMF
In bonding solvent and 2h is stirred, obtains uniform colloidal fluid, add 0.18g aniline ANI and 0.2245g camphorsulfonic acid CSA and is stirred
After mixing 2h, 0.4411g ammonium persulfates APS is added and simultaneously stirs 30min, then by mixed solution in ice-water bath magnetic agitation 2-3h
Afterwards, it is put into 5 DEG C of cold compartment of refrigerator for 24 hours, obtains spinning solution III;
(4) three function [(Fe of green fluorescence electromagnetism is prepared3O4/PVP)@(Tb(BA)3phen/PVP)]//[PANI/PVP]Janus
Nanofiber
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
Wire netting, other spinning parameters are:Spinning voltage is 13kV, and needle point is 16cm, environment temperature 20-26 with collecting net spacing
DEG C, relative humidity 20%-40% obtains three function [(Fe of green fluorescence electromagnetism3O4/PVP)@(Tb(BA)3phen/PVP)]//
[PANI/PVP] Janus nanofibers, by coaxial nano cable and nanofiber shoulder to shoulder and together with form, co-axial nano
The average diameter of cable and nanofiber is 600nm;Under the ultraviolet excitation of 276nm, [(Fe3O4/PVP)@(Tb(BA)3Phen/PVP)] // [PANI/PVP] Janus nanofibers launch the bright green light that main peak is located at 545nm;[(Fe3O4/
PVP)@(Tb(BA)3Phen/PVP)] // [PANI/PVP] average conductivity of Janus nanofibers is 1.460 × 10-4S·
cm-1;[(Fe3O4/PVP)@(Tb(BA)3Phen/PVP)] // [PANI/PVP] saturation magnetization of Janus nanofibers is
7.30emu/g, prepared special construction Janus nanofibers have the function of good green emitting-conduction-magnetism three.
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