CN107604497A - Magneto-optic double-function nano-fibre yams and preparation method thereof - Google Patents
Magneto-optic double-function nano-fibre yams and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to magneto-optic double-function nano-fibre yams 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 Eu (BA)3Phen complexs；(3) spinning solution is prepared；(4) [Fe is prepared3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams, prepared using conjugation single nozzle electrostatic spinning technique.Prepared nano-fibre yams have good magnetic and emitting red light difunctional simultaneously.The method of the present invention is simple for process, practical, non-environmental-pollution, can produce in batches, this new one-dimensional nano structure material has broad application prospects.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, in particulars relate to magneto-optic double-function nano-fibre yams and its system
Preparation Method.
Background technology
Simple function applications to nanostructures is limited in scope, and the application of dual-functional nanometer material is wider, this kind of material
Material has more characteristic and attraction, and therefore, dual-functional nanometer material is paid high attention to by researcher.With the hair of nanosecond science and technology
Exhibition, nano material are such as had the characteristics of luminescence, electric conductivity or magnetic, developed towards difunctional direction, such as had magnetic by simple function
Property-luminous, luminous-conductive or conduction-magnetic is difunctional, can so be realized on a kind of nano structural material it is difunctional, it is right
The development of the science and technology of nano-device, nanometer technology and correlation is significant.For example, magnetic-fluorescent dual-function is received
Nano composite material provides a kind of new platform for medical diagnosis on disease and treatment, because their difunctional property makes the " hair of disease
Existing-detection-treatment " is integrally formed, and the use of this nano composite material by the further efficiency for improving diagnosis and reduces secondary make
With causing the highest attention of researcher.Electromagnetism dual-functional nanometer compound is in thunderstorm activity, electromagnetic shielding, antistatic painting
Layer and sensor etc. have broad application prospects.Magneto-optic double-function nano-fibre yams, due to its unique performance, rich
Rich scientific meaning, wide application prospect and the important strategic status occupied in following nano structure device, in recent years
Cause the great attention of people.The report of magnetic and emitting red light dual-functional nanometer fiber yarn is had no at present.
Ferroso-ferric oxide Fe3O4It is a kind of important and wide variety of magnetic material.People use a variety of methods, such as
The methods of precipitation method, sol-gel process, microemulsion method, hydro-thermal and solvent-thermal method, thermal decomposition method, method of electrostatic spinning, successfully makes
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 europium complex Eu (BA)3Phen, Eu3+For europium ion, BA is benzoate anion, and phen is adjacent Féraud
Quinoline, turn into the red illuminating material of unique energy because of the unique electron configuration of europium ion, as luminous intensity is high, stability
Well, the advantages that fluorescence quantum yield is high, monochromaticjty is good, is a kind of wide variety of fluorescent material.Therefore, magnetic Fe is utilized3O4Receive
Meter Jing and rare-earth europium emitting complexes Eu (BA)3It is preferable thing that phen, which constructs the nano material with magneto-optic double-function characteristic,
Matter.
Existing research is it has been proved that work as dark colour magnetic Fe3O4Directly mix, can significantly reduce with rare earth compounding
Its illumination effect, therefore to obtain the good illumination effect of rare earth compounding, it is necessary to make rare earth compounding and Fe3O4Realize effective
Separation.If by Fe3O4It is nanocrystalline to be compounded to form nanofiber with polyacrylonitrile (PAN), by rare earth compounding Eu (BA)3Phen with
PAN is compounded to form nanofiber, and the twisting of both nanofibers is threaded together, forms nano-fibre yams, it is possible to realize
Fe3O4Efficiently separated with rare earth compounding, so as to obtain emitting red light of good performance-magnetic dual-functional nanometer fiber yarn, this
The new monodimension nanometer material of kind has not yet to see related document report by with important application prospect.
One relevant electrospinning process (electrospinning) of the U.S. Patent Publication of Patent No. 1975504
Technical scheme, this method is to prepare a kind of effective ways of micro nanometer fiber that is continuous, having 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 powered
Polymer Solution or melt are sprayed in electrostatic field by the traction of electrostatic force by nozzle, invest the receiving screen on opposite, so as to real
Existing wire drawing, then, solvent evaporates at normal temperatures, or melt cooling solidifies to normal temperature, obtains micro nanometer fiber.People are
Luminous and magnetic simple function, dual-functional nanometer fiber are prepared for using electrostatic spinning technique.Dong Xiangting etc. uses electrostatic spinning
Technology is prepared for the PAN/Eu (BA) with single lighting function3Phen luminous nano fibres film [New Chemical Materials, 2008,
36(9),49-52]；Wang Ce etc. is prepared for having magnetic polyvinylpyrrolidone/ferroso-ferric oxide multiple using method of electrostatic spinning
Close nano-fiber film [SCI, 2006,27 (10), 2002-2004]；Qingbiao Yang, et al. are adopted
Fe is prepared for electrostatic spinning technique2O3nanoparticles/Eu(DBM)3(Bath) compound difunctional magneto-optic nanofiber
[Journal of Colloid and Interface Science, 2010,350,396-401], Dong Xiangting etc. uses electrostatic
Spining technology is prepared for Fe3O4/Eu(BA)3Phen/PVP magneto-optic double-functions composite nano fiber [Journal of
Nanoparticle Research,2012,14(10):1203-1209]、Eu(BA)3Phen/PANI/PVP photoelectricity is difunctional multiple
Close nanofiber [SCI, 2012,33 (8), 1657-1662].Wu, et al. use electrostatic spinning technique system
For having the nano-fibre yams of high cell viability, this yarn is shown with the adhesion and propagation energy for improving cell
Power [ACS Appl.Mater.Interfaces, 2016,8,16950-16960]；Wang, et al. use electrostatic spinning technique
Be prepared for nano-fibre yams that PCL/silk fibroin/polyaniline align [ACS Nano, 2015,9,
9167-9179]；Before PAN is spun into nano-fibre yams so as to obtain carbon fiber by Xie, et al. by electrostatic spinning technique
Drive body [RSC Adv., 2015,5,15147-15153].At present, have no and prepare magnetic and emitting red light using electrostatic spinning technique
The relevant report of dual-functional nanometer fiber yarn.
When preparing nano material using electrostatic spinning technique, the species of raw material, the molecular weight of high polymer templates, spinning solution
Composition, the structure of spinning process parameter and spinning head all has a major impact to the pattern and size of final products.The present invention adopts
With conjugation single nozzle electrostatic spinning technique, two high-voltage DC power supplies are exported using positive high voltage output and negative high voltage, are driven by motor
Dynamic rotation brass bugle is twisted to fibre bundle, by the round metal bars of adjustable speed motor driving as collection device；By Eu (BA)3Phen and polyacrylonitrile (PAN) are added in DMF DMF, are configured to a Static Spinning with certain viscosity
Silk liquid, referred to as spinning solution I, by the Fe of Coated with Oleic Acid3O4Nanocrystalline, PAN and DMF mixing forms another spinning solution, referred to as spinning
Liquid II；Control the viscosity of spinning solution most important, under optimal process conditions, obtain the novel [Fe of structure3O4/PAN]//
[Eu(BA)3Phen/PAN] nano-fibre yams.
The content of the invention
Luminous and magnetic simple function, dual-functional nanometer fiber are prepared for using electrostatic spinning technique in the introduction,
The PAN nano fibre yarns of the nano-fibre yams and carbon fiber precursor for biological field are prepared for using electrostatic spinning technique
Line, used raw material, template, solvent and final target product and the method for the present invention are different.The present invention uses
Conjugation single nozzle electrostatic spinning technique is prepared for [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magnetic emitting red light is difunctional receives
Rice fiber yarn, a kind of nano-fiber material with novel characteristics is added for nanofiber field.
The present invention is achieved in for preparing Eu (BA) using the precipitation method first3Phen complexs and Coated with Oleic Acid
Fe3O4It is nanocrystalline, with Eu (BA)3The mixed liquor of phen complexs, PAN and DMF DMF is a kind of spinning solution,
Referred to as spinning solution I, by the Fe of Coated with Oleic Acid3O4Another spinning solution of nanocrystalline, PAN and DMF mixing compositions, referred to as spinning solution II,
The viscosity of spinning solution is controlled, electrostatic spinning is carried out using conjugation single nozzle electrostatic spinning technique, under optimal process conditions, obtained
Obtain [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams, its step is：
(1) precipitation method prepare the Fe of Coated with Oleic Acid3O4It is nanocrystalline
By 32.8500g FeCl3·6H2O, 16.7000g FeSO4·7H2O, 24.2400g NH4NO3With 11.4000g points
Son amount is dissolved in 600mL deionized waters for 20000 polyethylene glycol, is heated to 50 DEG C and is passed through argon gas 30min, is then slowly dripped
Ammonification water to the pH value of solution is 11, continues logical argon gas 20min and obtains black suspension, after this suspension Magneto separate, with nothing
Water-ethanol and deionized water are washed three times successively, and product is placed in 60 DEG C of vacuum drying chamber and dries 12h, obtains a diameter of 8-
10nm Fe3O4It is nanocrystalline；Take the Fe prepared by 2.0000g3O4It is nanocrystalline be dispersed in be passed through 30min argon gas 100mL go from
In sub- water and ultrasonic disperse 20min, solution is then heated to 80 DEG C under argon gas protection, and adds 1mL oleic acid, is then proceeded to
40min is reacted, resulting precipitation is subjected to Magneto separate, water layer is removed and will be deposited in 60 DEG C of vacuum drying chambers and dry 12h,
Obtain the Fe of Coated with Oleic Acid3O4It is nanocrystalline；
(2) precipitation method prepare Eu (BA)3Phen complexs
By 1.7600g Eu2O3Powder is dissolved in 20mL concentrated nitric acids, is heated to 120 DEG C, and the concentrated nitric acid of excess and water are steamed
Hair removes, and adds 20mL absolute ethyl alcohols, obtains Eu (NO3)3Ethanol solution, 3.6640g benzoic acid and 1.8020g is adjacent luxuriant and rich with fragrance
Sieve quinoline is dissolved in 200mL absolute ethyl alcohols jointly, then by Eu (NO3)3Ethanol solution be slowly added thereto, regulation pH 6-6.5 it
Between, 3h then is stirred at 60 DEG C, resulting precipitation deionized water and absolute ethyl alcohol alternately washing 6 times put product
12h is heated in 60 DEG C of baking ovens, obtains Eu (BA)3Phen powder；
(3) spinning solution is prepared
By 0.0750g Eu (BA)3Phen is added in 5.0000g DMF, and it is 86000 that 0.5000g molecular weight is added after dissolving
Polyacrylonitrile (PAN), magnetic agitation 3h at 60 DEG C, obtain spinning solution I；By the Fe of 0.9000g Coated with Oleic Acid3O4Nanocrystalline addition
Into 9.0000g DMF, ultrasonic disperse 20min, the polyacrylonitrile (PAN) that 0.9000g molecular weight is 86000 is added, in 60 DEG C
Lower stirring 3h is completely dissolved it, obtains spinning solution II；
(4) [Fe is prepared3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams
Using conjugation single nozzle electrostatic spinning technique, electrostatic spinning is carried out using two high-voltage DC power supplies, one is just
High-voltage DC power supply, positive high voltage is exported, another is negative high voltage dc source, negative high voltage is exported, by spinning solution I and spinning solution II
Pour into respectively in two 5mL plastic injectors with plastic spray gun head, electrode, one end of one section of copper cash are done respectively with two sections of copper cash
Insert in spinning solution I, the other end is connected with the positive high voltage output end of positive high voltage dc source, and one end insertion of another section of copper cash is spun
In silk liquid II, the other end is connected with the negative high voltage output end of negative high voltage dc source, with wire by positive and negative high-voltage DC power supply
Zero potential end is connected with ground wire respectively, plastic injector be positioned symmetrically in ground connection by it is motor-driven inversion brass bugle two
Side, the distance at loudspeaker Edge Distance lance head tip is 10cm, and when starting spinning, a metal is placed in the underface of loudspeaker
Silk, the taper fibre bundle of a handstand can be formed between the tip of wire and the edge of loudspeaker, by motor-driven rotation
Loudspeaker are twisted to fibre bundle, obtain nano-fibre yams, slowly downward drawing metal, yarn is drawn to by adjustable speed motor
For the round metal bars of driving as being collected on collection device, collection device round metal bars and the distance of loudspeaker lower end are 18cm,
Spinning voltage is ± 15kV, and loudspeaker rotating speed is 100r/min, and gathering speed 0.03m/min, environment temperature is 15-25 DEG C, phase
It is 15%-25% to humidity, obtains [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams.
Prepared [Fe in above process3O4/PAN]//[Eu(BA)3Phen/PAN] nano-fibre yams it is average straight
Footpath is 242 μm, by the Fe aligned3O4/ PAN magnetic Nanos fiber and Eu (BA)3Two kinds of phen/PAN fluorescent nano-fibers are not
Same nanofiber twisting forms, a diameter of 553 ± 2nm of nanofiber；Under 281nm ultraviolet excitation, [Fe3O4/
PAN]//[Eu(BA)3Phen/PAN] nano-fibre yams launch the bright red that main peak is located at 616nm；[Fe3O4/PAN]//
[Eu(BA)3Phen/PAN] saturation magnetizations of nano-fibre yams is 18.87emu/g, prepared [Fe3O4/PAN]//
[Eu(BA)3Phen/PAN] nano-fibre yams simultaneously have good magnetic and emitting red light difunctional, realize invention mesh
's.
Brief description of the drawings
Fig. 1 is [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams XRD spectra；
Fig. 2 is [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams SEM photograph, should
Figure also serves as Figure of abstract；
Fig. 3 is [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams high magnification SEM shine
Piece；
Fig. 4 is [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] nanofiber is straight in magneto-optic double-function nano-fibre yams
Footpath distribution histogram；
Fig. 5 is [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams EDS spectrograms；
Fig. 6 is [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams exciting light spectrogram；
Fig. 7 is [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams launching light spectrogram；
Fig. 8 is [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams hysteresis curve figure.
Embodiment
Europium oxide Eu selected by the present invention2O3Purity be 99.99%, benzoic acid, Phen, N, N- dimethyl methyls
Acid amides, Iron(III) chloride hexahydrate, green vitriol, ammonium nitrate, molecular weight be 20000 polyethylene glycol, nitric acid, molecular weight
It is commercially available analysis net product for 86000 polyacrylonitrile, absolute ethyl alcohol, ammoniacal liquor, oleic acid, argon gas；Deionized water laboratory is certainly
System；Glass apparatus and equipment used is the instrument and equipment commonly used in laboratory.
Embodiment：By 32.8500g FeCl3·6H2O, 16.7000g FeSO4·7H2O, 24.2400g NH4NO3With
The polyethylene glycol that 11.4000g molecular weight is 20000 is dissolved in 600mL deionized waters, is heated to 50 DEG C and is passed through argon gas 30min,
Then the pH value that ammoniacal liquor is slowly added dropwise to solution is 11, continues logical argon gas 20min and obtains black suspension, by this suspension magnetic point
From rear, washed successively three times with absolute ethyl alcohol and deionized water, product is placed in 60 DEG C of vacuum drying chamber and dries 12h, is obtained
To a diameter of 8-10nm Fe3O4It is nanocrystalline；Take the Fe prepared by 2.0000g3O4Nanocrystalline be dispersed in has been passed through 30min argon gas
100mL deionized waters in and ultrasonic disperse 20min, then by solution argon gas protection under be heated to 80 DEG C, and add 1mL oil
Acid, is then proceeded to react 40min, and resulting precipitation is carried out into Magneto separate, is removed water layer and will be deposited in 60 DEG C of vacuum drying
12h is dried in case, obtains the Fe of Coated with Oleic Acid3O4It is nanocrystalline；By 1.7600g Eu2O3Powder is dissolved in 20mL concentrated nitric acids, is added
The concentrated nitric acid of excess and water evaporation are removed to 120 DEG C, add 20mL absolute ethyl alcohols, obtain Eu (NO by heat3)3Ethanol it is molten
Liquid, 3.6640g benzoic acid and 1.8020g Phens are dissolved in 200mL absolute ethyl alcohols jointly, then by Eu (NO3)3Ethanol
Solution is slowly added thereto, and pH is between 6-6.5 for regulation, then 3h is stirred at 60 DEG C, by resulting precipitation deionization
Water and absolute ethyl alcohol alternately washing 6 times, product is placed in 60 DEG C of baking ovens and heats 12h, obtains Eu (BA)3Phen powder；Will
0.0750g Eu(BA)3Phen is added in 5.0000g DMF, and the polyacrylonitrile that 0.5000g molecular weight is 86000 is added after dissolving
PAN, magnetic agitation 3h at 60 DEG C, obtains spinning solution I；By the Fe of 0.9000g Coated with Oleic Acid3O4It is nanocrystalline to be added to 9.0000g
In DMF, ultrasonic disperse 20min adds the polyacrylonitrile (PAN) that 0.9000g molecular weight is 86000, and 3h is stirred at 60 DEG C to be made
It is completely dissolved, and obtains spinning solution II；Using conjugation single nozzle electrostatic spinning technique, carried out using two high-voltage DC power supplies quiet
Electrospun, one is positive high voltage dc source, exports positive high voltage, and another is negative high voltage dc source, exports negative high voltage, will spin
Silk liquid I and spinning solution II is poured into two 5mL plastic injectors with plastic spray gun head respectively, and electricity is done respectively with two sections of copper cash
Pole, one end of one section of copper cash are inserted in spinning solution I, and the other end is connected with the positive high voltage output end of positive high voltage dc source, another
In one end insertion spinning solution II of section copper cash, the other end is connected with the negative high voltage output end of negative high voltage dc source, will with wire
The zero potential end of positive and negative high-voltage DC power supply is connected with ground wire respectively, plastic injector be positioned symmetrically in ground connection by motor
The both sides of the inversion brass bugle of driving, the distance at loudspeaker Edge Distance lance head tip is 10cm, when starting spinning, in loudspeaker
An one metal wire is placed in underface, and the taper fiber of a handstand can be formed between the tip of wire and the edge of loudspeaker
Beam, twisted by motor-driven rotation loudspeaker to fibre bundle, nano-fibre yams are obtained, slowly downward drawing metal, by yarn
Line is drawn to the round metal bars by adjustable speed motor driving as being collected on collection device, collection device round metal bars and loudspeaker
The distance of lower end is 18cm, and spinning voltage is ± 15kV, and loudspeaker rotating speed is 100r/min, gathering speed 0.03m/min, ring
Border temperature is 15-25 DEG C, relative humidity 15%-25%, obtains [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] the double work(of magneto-optic
Can nano-fibre yams.Described [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] contain in magneto-optic double-function nano-fibre yams
There is Emission in Cubic Fe3O4It is nanocrystalline, as shown in Figure 1；Described [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function receives
The average diameter of rice fiber yarn is 242 μm, as shown in Figure 2；Described [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic
In dual-functional nanometer fiber yarn, the Fe aligned is included3O4/ PAN magnetic Nanos fiber and Eu (BA)3Phen/PAN fluorescence
Two kinds of different nanofibers of nanofiber, as shown in Figure 3；[Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function
A diameter of 553 ± 2nm of nanofiber in nano-fibre yams, as shown in Figure 4；[Fe3O4/PAN]//[Eu(BA)3phen/
PAN] by Fe, Eu, C, O, N composition, Pt derives to be led magneto-optic double-function nano-fibre yams with what surface during SEM observation samples was plated
Electrolemma, as shown in Figure 5；Monitoring wavelength, [Fe are used as using 616nm3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function receives
Rice fiber yarn has a wide excitation band at 200-350nm, and its peak value is located at 281nm, can be classified as π → π * jumps of part
Move, as shown in Figure 6；Under 281nm ultraviolet excitation, [Fe3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function receives
Rice fiber yarn launches the bright red that main peak is located at 616nm, and it corresponds to Eu ions5D0→7F2Transition, see Fig. 7 institutes
Show；Made [the Fe stated3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams have stronger magnetic,
Saturation magnetization is 18.87emu/g, as shown in Figure 8.
Certainly, the present invention can also have other various embodiments, ripe in the case of without departing substantially from spirit of the invention and its essence
Know those skilled in the art when can be made according to the present invention it is various it is corresponding change and deformation, but these corresponding change and become
Shape should all belong to the protection domain of appended claims of the invention.
Claims (2)
1. magneto-optic double-function nano-fibre yams, it is characterised in that by the Fe aligned3O4/ PAN magnetic Nanos fiber and Eu
(BA)3The different nanofiber twisting of two kinds of phen/PAN fluorescent nano-fibers forms, and yarn has magnetic and red hair simultaneously
Light is difunctional, and the average diameter of yarn is 242 μm.
2. a kind of preparation method of magneto-optic double-function nano-fibre yams as claimed in claim 1, it is characterised in that using altogether
Yoke single nozzle electrostatic spinning technique, it is [Fe to prepare product3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function Nanowire
Yarn is tieed up, its step is：
(1) precipitation method prepare the Fe of Coated with Oleic Acid3O4It is nanocrystalline
By 32.8500g FeCl3·6H2O, 16.7000g FeSO4·7H2O, 24.2400g NH4NO3With 11.4000g molecular weight
It is dissolved in for 20000 polyethylene glycol in 600mL deionized waters, is heated to 50 DEG C and is passed through argon gas 30min, ammonia is then slowly added dropwise
Water to the pH value of solution is 11, continues logical argon gas 20min and obtains black suspension, after this suspension Magneto separate, with anhydrous second
Alcohol and deionized water are washed three times successively, and product is placed in 60 DEG C of vacuum drying chamber and dries 12h, obtains a diameter of 8-10nm
Fe3O4It is nanocrystalline；Take the Fe prepared by 2.0000g3O4It is nanocrystalline to be dispersed in the 100mL deionized waters for being passed through 30min argon gas
In and ultrasonic disperse 20min, solution is then heated to 80 DEG C under argon gas protection, and 1mL oleic acid is added, then proceedes to react
40min, resulting precipitation is subjected to Magneto separate, removes water layer and will be deposited in 60 DEG C of vacuum drying chambers and dry 12h, obtain
The Fe of Coated with Oleic Acid3O4It is nanocrystalline；
(2) precipitation method prepare Eu (BA)3Phen complexs
By 1.7600g Eu2O3Powder is dissolved in 20mL concentrated nitric acids, is heated to 120 DEG C, and the concentrated nitric acid of excess and water evaporation are removed
Go, add 20mL absolute ethyl alcohols, obtain Eu (NO3)3Ethanol solution, by 3.6640g benzoic acid and 1.8020g Phens
It is dissolved in jointly in 200mL absolute ethyl alcohols, then by Eu (NO3)3Ethanol solution be slowly added thereto, regulation pH between 6-6.5,
Then 3h is stirred at 60 DEG C, by resulting precipitation deionized water and absolute ethyl alcohol alternately washing 6 times, product is placed on 60
12h is heated in DEG C baking oven, obtains Eu (BA)3Phen powder；
(3) spinning solution is prepared
By 0.0750g Eu (BA)3Phen is added in 5.0000g DMF, added after dissolving 0.5000g molecular weight be 86000 it is poly-
Acrylonitrile PAN, magnetic agitation 3h at 60 DEG C, obtains spinning solution I；By the Fe of 0.9000g Coated with Oleic Acid3O4It is nanocrystalline to be added to
In 9.0000g DMF, ultrasonic disperse 20min, the polyacrylonitrile (PAN) that 0.9000g molecular weight is 86000 is added, at 60 DEG C
Stirring 3h is completely dissolved it, obtains spinning solution II；
(4) [Fe is prepared3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams
Using conjugation single nozzle electrostatic spinning technique, electrostatic spinning is carried out using two high-voltage DC power supplies, one is positive high voltage
Dc source, positive high voltage is exported, another is negative high voltage dc source, exports negative high voltage, and spinning solution I and spinning solution II is distinguished
Pour into two 5mL plastic injectors with plastic spray gun head, electrode, one end insertion of one section of copper cash are done respectively with two sections of copper cash
In spinning solution I, the other end is connected with the positive high voltage output end of positive high voltage dc source, one end insertion spinning solution of another section of copper cash
In II, the other end is connected with the negative high voltage output end of negative high voltage dc source, electric by the zero of positive and negative high-voltage DC power supply with wire
Gesture end is connected with ground wire respectively, and plastic injector is positioned symmetrically in the both sides by motor-driven inversion brass bugle of ground connection,
The distance at loudspeaker Edge Distance lance head tip is 10cm, and when starting spinning, an one metal wire is placed in the underface of loudspeaker,
The taper fibre bundle of a handstand can be formed between the tip of wire and the edge of loudspeaker, is given by motor-driven rotation loudspeaker
Fibre bundle is twisted, and obtains nano-fibre yams, slowly downward drawing metal, and yarn is drawn to by adjustable speed motor driving
Round metal bars on collection device as being collected, and the distance of collection device round metal bars and loudspeaker lower end is 18cm, and spinning is electric
It is 100r/min to press as ± 15kV, loudspeaker rotating speed, and gathering speed 0.03m/min, environment temperature is 15-25 DEG C, relative humidity
For 15%-25%, [Fe is obtained3O4/PAN]//[Eu(BA)3Phen/PAN] magneto-optic double-function nano-fibre yams, average diameter
For 242 μm, by the Fe aligned3O4/ PAN magnetic Nanos fiber and Eu (BA)3Two kinds of differences of phen/PAN fluorescent nano-fibers
Nanofiber twisting form, a diameter of 553 ± 2nm of nanofiber, under 281nm ultraviolet excitation, [Fe3O4/
PAN]//[Eu(BA)3Phen/PAN] nano-fibre yams launch the bright red that main peak is located at 616nm, [Fe3O4/PAN]//
[Eu(BA)3Phen/PAN] saturation magnetizations of nano-fibre yams is 18.87emu/g, prepared [Fe3O4/PAN]//
[Eu(BA)3Phen/PAN] nano-fibre yams simultaneously have good magnetic and emitting red light difunctional.
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