CN109706621A - Anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film - Google Patents
Anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film Download PDFInfo
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Abstract
The present invention relates to anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite films, belong to technical field of nanometer material preparation.The present invention includes five steps: (1) precipitation method preparation Eu (BA)3Phen and Tb (BA)3Phen complex；(2) precipitation method prepare the Fe of Coated with Oleic Acid3O4It is nanocrystalline；(3) polymetylmethacrylate is prepared；(4) spinning solution is prepared；(5) anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film is prepared, is prepared using electrostatic spinning technique.Prepared flexible sandwich structure composite membrane has good anisotropic conductive magnetism red and green color fluorescent multifunctional characteristic simultaneously.Of the invention preparation method is simple, practical, can produce in batches, and this novel nano structural material has broad application prospects.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, in particular relate to anisotropic conductive magnetism red and green color fluorescence
Sandwich structure multifunctional composite film.
Background technique
Anisotropic conductive film is a kind of novel electronic component interconnecting material, it have electric conductivity in one direction and
Insulating properties on other directions, be widely used in Electronic Packaging, chip is fixed and electrode bonding etc. fields.It is led by it
Electric direction classification, can be divided into following two class: I type anisotropic conductive film: this anisotropic conductive film is along the thickness side of film
It to conduction, and insulate along film surface direction, the technology of preparing of this anisotropic conductive film is highly developed, and by widely
Using in the electronic device；II type anisotropic conductive film: this anisotropic conductive film has not along the different directions of its film surface
With electric conductivity, usually in two vertical direction of film surface, a direction conduction, another direction insulation, have it is each to
Anisotropic electric conductivity.The research of II type anisotropic conductive film is still in the laboratory exploratory stage, be not implemented industrialized production and
Using.The novel anisotropic conductive film of research and probe, and its multi-functional characteristic is assigned, it is anisotropic conductive film research field
Important development direction.
Janus material refers 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, fluorescence/conduction etc. is materials science field
One of forward position, hot research direction.Janus nanobelt refers to that two kinds of chemical compositions have clear subregion knot in same nanobelt
Structure has two or more property, and if the side of nanobelt has fluorescent functional, the other side of nanobelt has conductive function
Can, if these Janus nanobelts can align using special reception device, Janus nano-band array film is formed,
This array films have fluorescence and conduction difunctional.
Rare earth metal europium complex Eu (BA)3Phen and terbium coordination compound Tb (BA)3Phen, Eu3+And Tb3+Respectively europium ion
And terbium ion, BA are benzoic acid, phen is phenanthroline, become because of europium ion and the unique electron configuration of terbium ion have it is only
The red and green luminescent material of characteristic energy, such as luminous intensity is high, stability is good, fluorescence quantum yield is high, monochromaticjty is good excellent
Point is two kinds of widely applied red and green fluorescent materials.Polyaniline PANI is since it is readily synthesized, conductivity is high and environment
The advantages that stability is good has become one of the hot spot of conducting polymer area research.People have synthesized nano wire, nanometer
The polyaniline PANI of the one-dimensional nano structures such as stick, nanotube and nanofiber.
Existing research is it has been proved that as dark colour electrically conductive polyaniline PANI and rare earth compounding Eu (BA)3Phen is straight
Its illumination effect can be significantly reduced by connecing mixing, therefore obtain Eu (BA)3The good illumination effect of phen, it is necessary to make Eu (BA)3Phen and PANI realization efficiently separates.If conductive polymer polyanilinc PANI mixed with polymetylmethacrylate
Be prepared into nanobelt, conductive PANI be it is continuous, ensure that its high conductivity, as the side of Janus nanobelt, then the side
It is conductive, and by Eu (BA)3Phen, which is scattered in macromolecule PMMA, is prepared into nanobelt, as the another of Janus nanobelt
Side, then the side has red light-emitting characteristics, forms [PANI/PMMA] // [Eu (BA)3Phen/PMMA] emitting red light conductive pair
Function Janus nanobelt, so as to so that electrically conductive polyaniline PANI and Eu (BA)3Phen, which is realized, to be efficiently separated, and is obtained good
Illumination effect；If using special device Janus nano-band array film can also be obtained, in this way along nanometer strip length side
It is strong to electric conductivity, and along perpendicular on nanobelt direction, due to there is nonconducting Eu (BA)3Phen/PMMA structural unit is deposited
So that the direction has insulating properties, to have anisotropic conductive, [PANI/PMMA] // [Eu can be obtained by this way
(BA)3Phen/PMMA] anisotropic conductive red fluorescence Janus nano-band array film, secondary electrospinning is recycled,
Unordered Fe is constructed on Janus nano-band array film3O4/ polyvinylpyrrolidone PVP composite nano-fiber membrane has magnetism,
Electrospinning constructs unordered Tb (BA) to recycling on magnetic film three times3Phen/ polyacrylonitrile (PAN) composite nano-fiber membrane,
It has the function of green fluorescence, this trilamellar membrane is firmly combined together to form upper, middle and lower three-decker, obtains sandwich structure
Composite membrane, this sandwich structure composite membrane have anisotropic conductive magnetism red and green color fluorescent multifunctional characteristic, will be not
Come with important application prospects in nano structure device and medical diagnosis treatment.Have 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 a kind of effective ways for preparing 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 is sprayed by the traction of electrostatic force by nozzle in electrostatic field, invests the receiving screen on opposite, thus real
Existing wire drawing, then, solvent evaporation or melt are cooled to room temperature and solidify at normal temperature, obtain micro nanometer fiber.Nearly more than ten years
Since, occur preparing inorganic compound such as oxidate nano fibre using electrospinning process in inorfil preparation technical field
The technical solution of dimension, the oxide include TiO2、ZrO2、Y2O3、Y2O3:RE3+(RE3+=Eu3+、Tb3+、Er3+、Yb3+/Er3 +)、NiO、Co3O4、Mn2O3、Mn3O4、CuO、SiO2、Al2O3、V2O5、ZnO、Nb2O5、MoO3、CeO2、LaMO3(M=Fe, Cr, Mn,
Co、Ni、Al)、Y3Al5O12、La2Zr2O7Equal metal oxides and composite oxide of metal.Q.Z.Yu, et al. use Static Spinning
Silk technology is prepared for polyaniline PANI nanofiber [Mater.Sci.Eng.B, 2008,150,70-76].Someone utilizes electrostatic
Spining technology is successfully prepared high molecular nanometer band [Materials Letters, 2007,61:2325-2328；Journal of
Polymer Science:Part B:Polymer Physics,2001,39:2598-2606].Someone is organised using tin
Object is closed, is combined using electrostatic spinning technique with metallo-organic compound decomposition technique and is prepared for porous SnO2Nanobelt
[Nanotechnology,2007,18:435704].It is multiple that someone is prepared for PEO/ stannic hydroxide using electrostatic spinning technique first
Nanobelt is closed, is roasted to have obtained porous SnO2Nanobelt [J.Am.Ceram.Soc., 2008,91 (1): 257-262].Dong
Phase court of a feudal ruler etc. using electrostatic spinning technique be prepared for trifluorides nanobelt [Chinese invention patent, application number:
201010108039.7], titanium dioxide nano-belts [Chinese invention patent, grant number: ZL200810050948.2] and
Gd3Ga5O12:Eu3+Porous nano-belt [Chemical Journal of Chinese Universities, 2010,31 (7), 1291-1296].Dong Xiangting etc. uses single
A spinning head is prepared for PAN/Eu (BA) using electrostatic spinning technique3Phen recombination luminescence nanofiber [New Chemical Materials,
2008,36(9),49-52].Wang Ce etc. is prepared for having magnetic polyvinylpyrrolidone/tetra- oxidations three using method of electrostatic spinning
Iron composite nano-fiber film [Chemical Journal of Chinese Universities, 2006,27 (10), 2002-2004]；Qingbiao Yang,et
Al. Fe is prepared for using electrostatic spinning technique2O3nanoparticles/Eu(DBM)3(Bath) compound difunctional magneto-optic Nanowire
It ties up [Journal of Colloid and Interface Science, 2010,350,396-401].Dong Xiangting etc. uses single
A spinning head is prepared for Eu (BA) using electrostatic spinning technique3The difunctional composite nano fiber of phen/PANI/PVP photoelectricity is [high
Equal schools' chemistry journal, 2012,33 (8), 1657-1662].Dong Xiangting etc. is prepared for Eu (BA) using electrostatic spinning technique3Phen/PVP//PANI/PVP photoelectricity double function two-stranded parallel nanometer fiber bundle [national inventing patent, application number:
201210407369.5].Dong Xiangting etc. is prepared for the magnetic-light three functions Janus of single anisotropic conductive-using electrostatic spinning technique
Nano-band array [national inventing patent, grant number: ZL201410795673.0；Adv.Funct.Mater.,2015,25,
2436-2443].Dong Xiangting etc. is prepared for emitting red light electromagnetism three functions, two layers of composite nano-fiber membrane using electrostatic spinning technique
[national inventing patent, grant number: ZL201610765900.4；ACS Applied Materials&Interfaces,2016,8
(39),26226-26234].Currently, having no that prepare flexible anisotropic electroconductive magnetic red and green color using electrostatic spinning technique glimmering
The relevant report of light sandwich structure multifunctional composite film.
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 adopts
With electrostatic spinning technique, spinning head be close together by the identical syringe needle of two truncated diameters of 12# form it is arranged side by side double
Spinning head, by aniline, camphorsulfonic acid, ammonium persulfate, PMMA, n,N-Dimethylformamide DMF and chloroform CHCl3Mixing, to benzene
Amine constitutes the first spinning solution after aggregating into polyaniline, with Eu (BA)3Phen complex, PMMA, DMF and CHCl3Mixed liquor be
Second of spinning solution, with the Fe of Coated with Oleic Acid3O4The mixed liquor of nanocrystalline, PVP and DMF is the third spinning solution, Tb (BA)3The mixed liquor of phen complex, PAN and DMF is the 4th kind of spinning solution, and the viscosity for controlling spinning solution is most important, optimal
Under process conditions, [PANI/PMMA] // [Eu (BA) is obtained3Phen/PMMA] anisotropic conductive red fluorescence Janus nanobelt
Array films recycle secondary electrospinning, construct unordered Fe on Janus nano-band array film3O4/ PVP composite nano fiber
Magnetic film, electrospinning constructs unordered Tb (BA) to recycling on magnetic film three times3Phen/PAN composite nano fiber green
Fluorescent film, this trilamellar membrane are firmly combined together to form upper, middle and lower three-decker, obtain sandwich structure composite membrane, and this three
Mingzhi's structure composite film has anisotropic conductive magnetism red and green color fluorescent multifunctional characteristic.
Summary of the invention
Macromolecule, metal oxide, metal fluoride and metal are prepared for using electrostatic spinning technique in the background technology
Composite oxides nanofiber and nanobelt, PAN/Eu (BA)3Phen recombination luminescence nanofiber, polyvinylpyrrolidone/tetra-
Fe 3 O composite magnetic nanofiber, polyaniline PANI nanofiber, Eu (BA)3Phen/PANI/PVP photoelectricity is difunctional multiple
Close nanofiber, Eu (BA)3Phen/PVP//PANI/PVP photoelectricity double function two-stranded parallel nanometer fiber bundle, single anisotropy are led
Electricity-magnetic-light three functions Janus nano-band array and emitting red light electromagnetism three functions, two layers of composite nano-fiber membrane.It is used
Raw material, template, solvent and final target product and method of the invention are different.The present invention uses electrostatic spinning skill
Art is prepared for [PANI/PMMA] // [Eu (BA) using double-spinneret arranged side by side3Phen/PMMA] anisotropic conductive red fluorescence
Janus nano-band array film, recycles secondary electrospinning, constructs unordered Fe on Janus nano-band array film3O4/PVP
Composite nano fiber magnetic film, electrospinning constructs unordered Tb (BA) to recycling on magnetic film three times3Phen/PAN is compound
Nanofiber green fluorescent membrane, this trilamellar membrane are firmly combined together to form upper, middle and lower three-decker, obtain sandwich structure
Composite membrane increases a kind of new structural multi-functional anisotropic conductive film for anisotropic conductive film Material Field.
The invention is realized in this way preparing Eu (BA) using the precipitation method first3Phen and Tb (BA)3Phen complex
And the Fe of Coated with Oleic Acid3O4It is nanocrystalline, using mass polymerization prepare PMMA, by aniline, camphorsulfonic acid, ammonium persulfate,
PMMA, N,N-dimethylformamide DMF and chloroform CHCl3Mixing, constitutes the first spinning after aniline polymerization is at polyaniline PANI
Silk liquid, with Eu (BA)3Phen complex, PMMA, DMF and CHCl3Mixed liquor be second of spinning solution, with Coated with Oleic Acid
Fe3O4The mixed liquor of nanocrystalline, PVP and DMF is the third spinning solution, Tb (BA)3The mixed liquor of phen complex, PAN and DMF
For the 4th kind of spinning solution, the viscosity for controlling spinning solution is most important.It is carried out using double-spinneret arranged side by side, using electrostatic spinning technique
Electrostatic spinning obtains [PANI/PMMA] // [Eu (BA) under optimal process conditions3Phen/PMMA] anisotropic conductive is red
Color fluorescence Janus nano-band array film, recycles secondary electrospinning, constructs on Janus nano-band array film unordered
Fe3O4/ PVP composite nano fiber magnetic film, electrospinning constructs unordered Tb (BA) to recycling on magnetic film three times3phen/
PAN composite nano fiber green fluorescent membrane, this trilamellar membrane are firmly combined together to form upper, middle and lower three-decker, obtain Sanming City
Control structure composite film.It the steps include:
(1) precipitation method preparation Eu (BA)3Phen and Tb (BA)3Phen complex
By 1.7600g Eu2O3It is dissolved in 20mL concentrated nitric acid, heating is evaporated to obtain Eu (NO3)3It is anhydrous that 20mL is added in crystal
Ethyl alcohol is configured to Eu (NO3)3Ethanol solution；It is anhydrous that 3.6640g benzoic acid and 1.8020g phenanthroline are added to 200mL
Mixed ligand solution is configured in ethyl alcohol, in the case where being stirred continuously by Eu (NO3)3Ethanol solution be added dropwise to mixing and match
In liquid solution, dense NH is added3·H2O adjusts pH between 6.5-7.0, after being heated to 60 DEG C, reacts 3h, gained precipitates successively
With water and ethanol washing 3 times, 12h is finally dried at 60 DEG C in drying box, obtains Eu (BA)3Phen complex；By 1.8650g
Tb4O7It is dissolved in 15mL concentrated nitric acid, heating is evaporated to obtain Tb (NO3)3Crystal is added 20mL dehydrated alcohol, is configured to Tb (NO3)3
Ethanol solution；3.6640g benzoic acid and 1.8000g phenanthroline are added in 200mL dehydrated alcohol to be configured to mix and matched
Liquid solution, in the case where being stirred continuously by Tb (NO3)3Ethanol solution be added dropwise in mixed ligand solution, add dense
NH3·H2O adjusts pH between 6.5-7.0, after being heated to 60 DEG C, reacts 3h, and gained precipitating successively uses water and ethanol washing 3 times,
12h is finally dried at 60 DEG C in drying box, obtains Tb (BA)3Phen complex；
(2) 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 water for 20000 polyethylene glycol, is heated to 50 DEG C and is passed through argon gas 30min, is then slowly dripped
The pH value for adding ammonium hydroxide to 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 successively washed three times, and place the product in 12h dry in 60 DEG C of vacuum oven, and obtaining diameter is 8-
The Fe of 10nm3O4It is nanocrystalline；Take 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, then solution is heated to 80 DEG C, and 1mL oleic acid is added under protection of argon gas, then proceeded to
40min is reacted, obtained precipitating is subjected to Magneto separate, remove water layer and dry 12h will be deposited in 60 DEG C of vacuum ovens,
Obtain the Fe of Coated with Oleic Acid3O4It is nanocrystalline；
(3) polymetylmethacrylate is prepared
100g methyl methacrylate MMA and 0.1g dibenzoyl peroxide BPO is weighed, is added to reflux unit
In 250mL three-necked bottle and stir evenly, by above-mentioned solution 90-95 DEG C at a temperature of be vigorously stirred and be back to solution and have centainly
Viscosity stops heating and naturally cools to room temperature after its viscosity is close with glycerol while continuing stirring, later will be above-mentioned
Infusion is into test tube, influx height 5-7cm, and 2h is stood after perfusion to invisible spectro solution does not have bubble, then
Above-mentioned test tube is transferred in 50 DEG C of drying boxes and places 48h, invisible spectro liquid hardening is transparent solid, finally by drying box
Temperature improves to 110 DEG C and keeps the temperature 2h, terminates polymerization reaction, then cooled to room temperature, obtains poly-methyl methacrylate
Ester PMMA；
(4) spinning solution is prepared
In 16.0000g CHCl31.0000g PMMA is added with the in the mixed solvent of 0.5000g DMF, stirring 2h is obtained
0.7000g aniline and 1.7596g camphorsulfonic acid are added in above-mentioned colloidal fluid and after stirring 2h by uniform colloidal fluid, are added
1.7153g ammonium persulfate adds 1.5000g CHCl3Solution is put into 5 DEG C of refrigerator after stirring 2h with 1.000g DMF
In refrigerating chamber for 24 hours, the first spinning solution is obtained；It is added in the in the mixed solvent of 17.5000g chloroform and 1.5000g DMF
1.0000g PMMA and 0.15000g Eu (BA)3Phen complex simultaneously stirs for 24 hours, obtains second of spinning solution；In 4.8000g
The Fe of 1.0000g Coated with Oleic Acid is added in DMF solvent3O4Nanocrystalline, after ultrasonic disperse 20min, 1.0000g molecular weight, which is added, is
1300000 PVP is simultaneously stirred for 24 hours, obtains the third spinning solution；1.0000g molecular weight is added in 10.0000g DMF solvent
For 86000 PAN and 0.15000g Tb (BA)3Phen complex simultaneously stirs for 24 hours, obtains the 4th kind of spinning solution；
(5) anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film is prepared
The 5mL syringe that truncated 12# stainless steel syringe needle is all had using two difference is distinguished two stainless pin heads curved
Bent 30 ° of angles keep two needle points closely parallel, and make on two parallel stainless steel syringe needles using a 1mL plastic spray gun headgear
The tip of two stainless steel syringe needles is in the middle section of plastic spray gun head, the first spinning solution and second of spinning solution are respectively taken
2.5mL is injected separately into two syringes, and using perpendicular spray mode, reception device is a horizontal positioned long 20cm, diameter
For the cylindrical aluminum rotating cylinder of 7cm, revolving speed 1200r/min, other spinning parameters are as follows: spinning voltage 7kV, needle point and rotating cylinder
Spacing is 14cm, and environment temperature is 20-25 DEG C, and relative humidity 20%-30% obtains [PANI/ after spinning solution exhausts
PMMA]//[Eu(BA)3Phen/PMMA] anisotropic conductive red fluorescence Janus nano-band array film；The Janus that will be obtained
Nano-band array film is removed from aluminum rotating cylinder, is fixed on the wire netting being connected with high voltage power supply cathode, by the third of 5mL
Spinning solution is injected into the syringe with stainless steel syringe needle, using uniaxial electrospinning technology, in Janus nano-band array film
On construct unordered Fe3O4/ PVP composite nano fiber magnetic film, spinning parameter are as follows: spinning voltage 14kV, needle point and collection iron wire
Net spacing 16cm, environment temperature are 23-26 DEG C, relative humidity 20%-30%；After the third spinning solution is completely depleted, 5mL
Four kinds of spinning solutions replace the third spinning solution to continue spinning, and unordered Tb (BA) is constructed on magnetic film3Phen/PAN is compound to be received
Rice fiber green fluorescent membrane, this trilamellar membrane are firmly combined together to form upper, middle and lower three-decker, obtain anisotropic conductive
Magnetic red and green color fluorescence sandwich structure multifunctional composite film.
Prepared anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film in the above process,
By [PANI/PMMA] // [Eu (BA)3Phen/PMMA] it is anisotropic conductive red fluorescence Janus nano-band array film, unordered
Fe3O4/ PVP composite nano fiber magnetic film and unordered Tb (BA)3Phen/PAN composite nano fiber green fluorescent membrane it is compound and
At formation upper, middle and lower three-decker, the thickness of upper, middle and lower trilamellar membrane is respectively 46.15,39.56 and 65.36 μm, and lower membrane is by fixed
To [PANI/PMMA] // [Eu (BA) of arrangement3Phen/PMMA] Janus nanobelt composition, the width of Janus nanobelt is
10.25 ± 0.3 μm, strong along Janus nanobelt length direction electric conductivity, conductance is 7.62 × 10-2S, and along perpendicular to
Janus nanobelt length direction electric conductivity is weak, and conductance is 3.36 × 10-10S, the two ratio are 2.27 × 108, there is by force each
Anisotropy electric conductivity, under the ultraviolet excitation of 290nm, lower membrane launches the bright red that main peak is located at 615nm；Mesopelagic layer
By unordered magnetic Fe3O4/ PVP composite nano fiber composition, diameter are 480 ± 3nm；Upper layer film is by unordered Tb (BA)3Phen/PAN composite nano fiber composition, diameter are 630 ± 5nm, and under the ultraviolet excitation of 314nm, upper layer film launches master
Peak is located at the bright green light of 545nm；The saturation magnetization of prepared sandwich structure composite membrane is 5.14emu/g, is had
Stronger magnetism；Prepared flexible sandwich structure composite membrane has good anisotropic conductive magnetism red and green color fluorescence
Multi-functional characteristic, realizes goal of the invention.
Detailed description of the invention
Fig. 1 is the SEM photograph of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film, the figure
Also serve as Figure of abstract；
Fig. 2 is the XRD diagram of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film；
Fig. 3 is the SEM of the lower membrane of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film
Photo；
Fig. 4 is in the lower membrane of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film
The width distribution histogram of Janus nanobelt；
Fig. 5 is in the lower membrane of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film
The line analysis energy dispersion spectrogram of Janus nanobelt；
Fig. 6 is single in the lower membrane of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film
The optical microscope photograph of Janus nanobelt；
Fig. 7 is the transmitting of the lower membrane of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film
Spectrogram；
Fig. 8 is that the color of the lower membrane of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film is sat
It marks on a map；
Fig. 9 is the SEM of the mesopelagic layer of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film
Photo；
Figure 10 be anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film mesopelagic layer in receive
The diameter distribution histogram of rice fiber；
Figure 11 is the SEM of the upper layer film of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film
Photo；
Figure 12 be anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film upper layer film in receive
The diameter distribution histogram of rice fiber；
Figure 13 is the hair of the upper layer film of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film
Penetrate spectrogram；
Figure 14 is the color of the upper layer film of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film
Coordinate diagram；
Figure 15 is the hysteresis loop figure of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film.
Specific embodiment
Europium oxide Eu selected by the present invention2O3With terbium oxide Tb4O7Purity be 99.99%, N, N- dimethyl formyl
Amine, chloroform, nitric acid, benzoic acid, phenanthroline, dehydrated alcohol, ammonium hydroxide, aniline, camphorsulfonic acid, dibenzoyl peroxide, methyl
Methyl acrylate, ammonium persulfate, Iron(III) chloride hexahydrate, green vitriol, ammonium nitrate, the poly- second that molecular weight is 20000
Glycol, oleic acid, argon gas, the polyacrylonitrile (PAN) that molecular weight is 86000, the polyvinylpyrrolidone PVP that molecular weight is 1300000,
It is commercially available analysis net product；The self-control of deionized water laboratory；Glass apparatus and equipment used is common instrument in laboratory
Device and equipment.
Embodiment: by 1.7600g Eu2O3It is dissolved in 20mL concentrated nitric acid, heating is evaporated to obtain Eu (NO3)3Crystal is added
20mL dehydrated alcohol is configured to Eu (NO3)3Ethanol solution；3.6640g benzoic acid and 1.8020g phenanthroline are added to
Mixed ligand solution is configured in 200mL dehydrated alcohol, in the case where being stirred continuously by Eu (NO3)3Ethanol solution add dropwise
Into mixed ligand solution, dense NH is added3·H2O adjusts pH between 6.5-7.0, after being heated to 60 DEG C, reacts 3h, gained
Precipitating successively uses water and ethanol washing 3 times, finally dries 12h at 60 DEG C in drying box, obtains Eu (BA)3Phen complex；
By 1.8650g Tb4O7It is dissolved in 15mL concentrated nitric acid, heating is evaporated to obtain Tb (NO3)320mL dehydrated alcohol is added in crystal, prepares
At Tb (NO3)3Ethanol solution；3.6640g benzoic acid and 1.8000g phenanthroline are added in 200mL dehydrated alcohol and prepared
At mixed ligand solution, in the case where being stirred continuously by Tb (NO3)3Ethanol solution be added dropwise in mixed ligand solution, then
Dense NH is added3·H2O adjusts pH between 6.5-7.0, after being heated to 60 DEG C, reacts 3h, gained precipitating is successively washed with water and ethyl alcohol
It washs 3 times, finally dries 12h at 60 DEG C in drying box, obtain Tb (BA)3Phen complex；By 32.8500g FeCl3·
6H2O, 16.7000g FeSO4·7H2O, 24.2400g NH4NO3The polyethylene glycol for being 20000 with 11.4000g molecular weight is dissolved in
In 600mL deionized water, it is heated to 50 DEG C and is passed through argon gas 30min, the pH value that ammonium hydroxide is then slowly added dropwise to solution is 11, after
Continuous logical argon gas 20min obtains black suspension, after this suspension Magneto separate, successively washs three with dehydrated alcohol and deionized water
Secondary, place the product in 12h dry in 60 DEG C of vacuum oven, obtain the Fe that diameter is 8-10nm3O4It is nanocrystalline；Take 2.0000g
Prepared Fe3O4It is nanocrystalline to be dispersed in the 100mL deionized water for be passed through 30min argon gas simultaneously ultrasonic disperse 20min, then
Solution is heated to 80 DEG C under protection of argon gas, and 1mL oleic acid is added, then proceed to reaction 40min, by it is obtained precipitate into
Row Magneto separate removes water layer and will be deposited in 60 DEG C of vacuum ovens dry 12h, obtains the Fe of Coated with Oleic Acid3O4It is nanocrystalline；
100g methyl methacrylate MMA and 0.1g dibenzoyl peroxide BPO is weighed, the 250mL tri- with reflux unit is added to
In neck bottle and stir evenly, by above-mentioned solution 90-95 DEG C at a temperature of be vigorously stirred and be back to solution and have certain viscosity, when
After its viscosity is close with glycerol, stops heating while continuing stirring and naturally cool to room temperature, later fill above-mentioned solution
It infuses in test tube, influx height 5-7cm, 2h is stood after perfusion to invisible spectro solution does not have bubble, then will be above-mentioned
Test tube, which is transferred in 50 DEG C of drying boxes, places 48h, and invisible spectro liquid hardening is transparent solid, finally proposes drying box temperature
Up to 110 DEG C and 2h is kept the temperature, terminates polymerization reaction, then cooled to room temperature, obtain polymetylmethacrylate；
In 16.0000g CHCl31.0000g PMMA is added with the in the mixed solvent of 0.5000g DMF, stirring 2h obtains uniform glue
0.7000g aniline and 1.7596g camphorsulfonic acid are added in above-mentioned colloidal fluid and after stirring 2h by shape liquid, and 1.7153g mistake is added
Ammonium sulfate adds 1.5000g CHCl3Solution is put into 5 DEG C of cold compartment of refrigerator after stirring 2h with 1.000g DMF
For 24 hours, the first spinning solution is obtained；1.0000g PMMA is added in the in the mixed solvent of 17.5000g chloroform and 1.5000g DMF
With 0.15000g Eu (BA)3Phen complex simultaneously stirs for 24 hours, obtains second of spinning solution；Add in 4.8000g DMF solvent
Enter the Fe of 1.0000g Coated with Oleic Acid3O4It is nanocrystalline, after ultrasonic disperse 20min, the PVP that 1.0000g molecular weight is 1300000 is added
And stir for 24 hours, obtain the third spinning solution；The PAN that 1.0000g molecular weight is 86000 is added in 10.0000g DMF solvent
With 0.15000g Tb (BA)3Phen complex simultaneously stirs for 24 hours, obtains the 4th kind of spinning solution；It is all had using two difference truncated
12# stainless steel syringe needle 5mL syringe, two stainless pin heads are bent 30 ° of angles respectively, keep two needle points closely parallel, and
Using a 1mL plastic spray gun headgear on two parallel stainless steel syringe needles, the tip of two stainless steel syringe needles is made to be in plastics
The first spinning solution and second of spinning solution are respectively taken 2.5mL to be injected separately into two syringes by the middle section of lance head,
Using perpendicular spray mode, reception device is a horizontal positioned long 20cm, and diameter is the cylindrical aluminum rotating cylinder of 7cm, and revolving speed is
1200r/min, other spinning parameters are as follows: spinning voltage 7kV, needle point and rotating cylinder spacing are 14cm, environment temperature 20-25
DEG C, relative humidity 20%-30% obtains [PANI/PMMA] // [Eu (BA) after spinning solution exhausts3Phen/PMMA] respectively to
Anisotropic conduction red fluorescence Janus nano-band array film；Obtained Janus nano-band array film is removed from aluminum rotating cylinder,
It is fixed on the wire netting being connected with high voltage power supply cathode, the third spinning solution of 5mL is injected into stainless steel syringe needle
In syringe, using uniaxial electrospinning technology, unordered Fe is constructed on Janus nano-band array film3O4/ PVP composite Nano
Fiber magnetic film, spinning parameter are as follows: spinning voltage 14kV, needle point and collection wire netting spacing 16cm, environment temperature 23-26
DEG C, relative humidity 20%-30%；After the third spinning solution is completely depleted, the 4th kind of spinning solution of 5mL replaces the third spinning solution
Continue spinning, unordered Tb (BA) is constructed on magnetic film3Phen/PAN composite nano fiber green fluorescent membrane, this trilamellar membrane jail
Admittedly be combined together to form upper, middle and lower three-decker, it is more to obtain anisotropic conductive magnetism red and green color fluorescence sandwich structure
Functional composite membrane.Prepared anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film, by
[PANI/PMMA]//[Eu(BA)3Phen/PMMA] anisotropic conductive red fluorescence Janus nano-band array film, Fe3O4/PVP
Composite nano fiber magnetic film and Tb (BA)3Phen/PAN composite nano fiber green fluorescent membrane is combined, and forms upper, middle and lower
Three-decker, the thickness of upper, middle and lower trilamellar membrane are respectively 46.15,39.56 and 65.36 μm, as shown in Figure 1；Anisotropic conductive
Contain cubic phase Fe in magnetic red and green color fluorescence sandwich structure multifunctional composite film3O4It is nanocrystalline, as shown in Figure 2；Sandwich
In structure multifunctional composite membrane, lower membrane is by [PANI/PMMA] // [Eu (BA) for aligning3Phen/PMMA] Janus nanometers
Band composition, as shown in Figure 3；The width of Janus nanobelt is 10.25 ± 0.3 μm in lower membrane, as shown in Figure 4；For each to different
The structure of Janus nanobelt, Eu and S in the lower membrane of property electroconductive magnetic red and green color fluorescence sandwich structure multifunctional composite film
The distribution of element can reflect Eu (BA) respectively3The distribution of phen and polyaniline, Eu element are distributed only over the one of Janus nanobelt
Side, S Elemental redistribution is in the other side of Janus nanobelt, this is consistent with the structure of Janus nanobelt, as shown in Figure 5；For
The knot of Janus nanobelt in the lower membrane of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film
Structure, the side of single Janus nanobelt include dark colour PANI/PAMM, and the other side includes colorless and transparent Eu (BA)3Phen/PMMA, as shown in Figure 6；Under the ultraviolet excitation of 290nm, lower membrane launches the bright red that main peak is located at 615nm
Light, it corresponds to Eu ion5D0→7F2Transition, as shown in Figure 7；Under the ultraviolet excitation of 290nm, lower membrane emits glimmering
Chromaticity coordinates the value x and y of light color are respectively 0.632 and 0.334, and the fluorescence color of transmitting is red, as shown in Figure 8；Lower membrane
In it is strong along Janus nanobelt length direction electric conductivity, conductance be 7.62 × 10-2S, and along perpendicular to Janus nanometers of belt lengths
It is weak to spend direction electric conductivity, conductance is 3.36 × 10-10S, the two ratio are 2.27 × 108, there is strong anisotropic conductive；
Mesopelagic layer is by unordered magnetic Fe3O4/ PVP composite nano fiber composition, as shown in Figure 9；Magnetic Fe in mesopelagic layer3O4/ PVP is multiple
The diameter for closing nanofiber is 480 ± 3nm, as shown in Figure 10；Upper layer film is by unordered Tb (BA)3Phen/PAN composite Nano is fine
Dimension composition, as shown in figure 11；Tb (BA) in upper layer film3The diameter of phen/PAN composite nano fiber is 630 ± 5nm, such as Figure 12
It is shown；Under the ultraviolet excitation of 314nm, upper layer film launches the bright green light that main peak is located at 545nm, it corresponds to Tb ion
's5D4→7F5Transition, as shown in figure 13；Under the ultraviolet excitation of 314nm, the chromaticity coordinates value of the fluorescence color of upper layer film transmitting
X and y is respectively 0.255 and 0.639, and the fluorescence color of transmitting is green, as shown in figure 14；Prepared anisotropic conductive magnetic
Property red and green color fluorescence sandwich structure multifunctional composite film saturation magnetization be 5.14emu/g, have stronger magnetism,
As shown in figure 15；Prepared sandwich structure composite membrane has the more function of good anisotropic conductive magnetism red and green color fluorescence
It can 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 changes and modifications, but these corresponding changes and change in accordance with the present invention
Shape all should fall within the scope of protection of the appended claims of the present invention.
Claims (2)
1. anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film, which is characterized in that by [PANI/
PMMA]//[Eu(BA)3Phen/PMMA] anisotropic conductive red fluorescence Janus nano-band array film, Fe3O4/ PVP is compound to be received
Rice fiber magnetic film and Tb (BA)3Phen/PAN composite nano fiber green fluorescent membrane is combined, and forms upper, middle and lower three-layered node
Structure, lower membrane is by [PANI/PMMA] // [Eu (BA) for aligning3Phen/PMMA] Janus nanobelt constitute, mesopelagic layer by
Unordered Fe3O4/ PVP composite nano fiber is constituted, and upper layer film is by unordered Tb (BA)3Phen/PAN composite nano fiber is constituted,
Trilamellar membrane is firmly combined together to form upper, middle and lower three-decker, obtains sandwich structure composite membrane, prepared sandwich
Structure composite film has good anisotropic conductive magnetism red and green color fluorescent multifunctional characteristic simultaneously.
2. a kind of anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film as described in claim 1
Preparation method, which is characterized in that use electrostatic spinning technique, prepare product be anisotropic conductive magnetism red and green color fluorescence
Sandwich structure multifunctional composite film, the steps include:
(1) precipitation method preparation Eu (BA)3Phen and Tb (BA)3Phen complex
By 1.7600g Eu2O3It is dissolved in 20mL concentrated nitric acid, heating is evaporated to obtain Eu (NO3)320mL dehydrated alcohol is added in crystal,
It is configured to Eu (NO3)3Ethanol solution；3.6640g benzoic acid and 1.8020g phenanthroline are added in 200mL dehydrated alcohol
It is configured to mixed ligand solution, in the case where being stirred continuously by Eu (NO3)3Ethanol solution be added dropwise to mixed ligand solution
In, add dense NH3·H2O adjust pH for 6.5-7.0 between, after being heated to 60 DEG C, react 3h, gained precipitating successively with water with
Ethanol washing 3 times, 12h is finally dried at 60 DEG C in drying box, obtains Eu (BA)3Phen complex；By 1.8650g Tb4O7
It is dissolved in 15mL concentrated nitric acid, heating is evaporated to obtain Tb (NO3)3Crystal is added 20mL dehydrated alcohol, is configured to Tb (NO3)3Second
Alcoholic solution；3.6640g benzoic acid and 1.8000g phenanthroline be added in 200mL dehydrated alcohol to be configured to mixed ligand molten
Liquid, in the case where being stirred continuously by Tb (NO3)3Ethanol solution be added dropwise in mixed ligand solution, add dense NH3·
H2O adjusts pH between 6.5-7.0, after being heated to 60 DEG C, reacts 3h, gained precipitating successively uses water and ethanol washing 3 times, finally
Dry 12h at 60 DEG C, obtains Tb (BA) in drying box3Phen complex；
(2) 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 600mL deionized water for 20000 polyethylene glycol, is heated to 50 DEG C and is passed through argon gas 30min, ammonia is then slowly added dropwise
The pH value of water to solution is 11, continues logical argon gas 20min and obtains black suspension, after this suspension Magneto separate, with anhydrous second
Pure and mild deionized water is successively washed three times, and place the product in 12h dry in 60 DEG C of vacuum oven, and obtaining diameter is 8-10nm
Fe3O4It is nanocrystalline；Take Fe prepared by 2.0000g3O4It is nanocrystalline to be dispersed in the 100mL deionized water for being passed through 30min argon gas
In and ultrasonic disperse 20min, then solution is heated to 80 DEG C, and 1mL oleic acid is added under protection of argon gas, then proceedes to react
Obtained precipitating is carried out Magneto separate by 40min, is removed water layer and will be deposited in 60 DEG C of vacuum ovens dry 12h, obtains
The Fe of Coated with Oleic Acid3O4It is nanocrystalline；
(3) polymetylmethacrylate is prepared
100g methyl methacrylate MMA and 0.1g dibenzoyl peroxide BPO is weighed, is added to reflux unit
In 250mL three-necked bottle and stir evenly, by above-mentioned solution 90-95 DEG C at a temperature of be vigorously stirred and be back to solution and have centainly
Viscosity stops heating and naturally cools to room temperature after its viscosity is close with glycerol while continuing stirring, later will be above-mentioned
Infusion is into test tube, influx height 5-7cm, and 2h is stood after perfusion to invisible spectro solution does not have bubble, then
Above-mentioned test tube is transferred in 50 DEG C of drying boxes and places 48h, invisible spectro liquid hardening is transparent solid, finally by drying box
Temperature improves to 110 DEG C and keeps the temperature 2h, terminates polymerization reaction, then cooled to room temperature, obtains poly-methyl methacrylate
Ester PMMA；
(4) spinning solution is prepared
In 16.0000g CHCl31.0000g PMMA is added with the in the mixed solvent of 0.5000g DMF, stirring 2h is obtained uniformly
0.7000g aniline and 1.7596g camphorsulfonic acid are added in above-mentioned colloidal fluid and after stirring 2h by colloidal fluid, and 1.7153g is added
Ammonium persulfate adds 1.5000g CHCl3Solution is put into 5 DEG C of cold compartment of refrigerator after stirring 2h with 1.000g DMF
For 24 hours, the first spinning solution is obtained；1.0000g PMMA is added in the in the mixed solvent of 17.5000g chloroform and 1.5000g DMF
With 0.15000g Eu (BA)3Phen complex simultaneously stirs for 24 hours, obtains second of spinning solution；Add in 4.8000g DMF solvent
Enter the Fe of 1.0000g Coated with Oleic Acid3O4It is nanocrystalline, after ultrasonic disperse 20min, the PVP that 1.0000g molecular weight is 1300000 is added
And stir for 24 hours, obtain the third spinning solution；The PAN that 1.0000g molecular weight is 86000 is added in 10.0000g DMF solvent
With 0.15000g Tb (BA)3Phen complex simultaneously stirs for 24 hours, obtains the 4th kind of spinning solution；
(5) anisotropic conductive magnetism red and green color fluorescence sandwich structure multifunctional composite film is prepared
The 5mL syringe that truncated 12# stainless steel syringe needle is all had using two difference, two stainless pin heads are bent respectively
30 ° of angles keep two needle points closely parallel, and make two on two parallel stainless steel syringe needles using a 1mL plastic spray gun headgear
The tip of root stainless steel syringe needle is in the middle section of plastic spray gun head, the first spinning solution and second of spinning solution are respectively taken
2.5mL is injected separately into two syringes, and using perpendicular spray mode, reception device is a horizontal positioned long 20cm, diameter
For the cylindrical aluminum rotating cylinder of 7cm, revolving speed 1200r/min, other spinning parameters are as follows: spinning voltage 7kV, needle point and rotating cylinder
Spacing is 14cm, and environment temperature is 20-25 DEG C, and relative humidity 20%-30% obtains [PANI/ after spinning solution exhausts
PMMA]//[Eu(BA)3Phen/PMMA] anisotropic conductive red fluorescence Janus nano-band array film；The Janus that will be obtained
Nano-band array film is removed from aluminum rotating cylinder, is fixed on the wire netting being connected with high voltage power supply cathode, by the third of 5mL
Spinning solution is injected into the syringe with stainless steel syringe needle, using uniaxial electrospinning technology, in Janus nano-band array film
On construct unordered Fe3O4/ PVP composite nano fiber magnetic film, spinning parameter are as follows: spinning voltage 14kV, needle point and collection iron wire
Net spacing 16cm, environment temperature are 23-26 DEG C, relative humidity 20%-30%；After the third spinning solution is completely depleted, 5mL
Four kinds of spinning solutions replace the third spinning solution to continue spinning, and unordered Tb (BA) is constructed on magnetic film3Phen/PAN is compound to be received
Rice fiber green fluorescent membrane, this trilamellar membrane are firmly combined together to form upper, middle and lower three-decker, obtain anisotropic conductive
Magnetic red and green color fluorescence sandwich structure multifunctional composite film, by [PANI/PMMA] // [Eu (BA)3Phen/PMMA] respectively to
Anisotropic conduction red fluorescence Janus nano-band array film, unordered Fe3O4/ PVP composite nano fiber magnetic film and unordered Tb
(BA)3Phen/PAN composite nano fiber green fluorescent membrane is combined, and forms upper, middle and lower three-decker, upper, middle and lower trilamellar membrane
Thickness is respectively 46.15,39.56 and 65.36 μm, and lower membrane is by [PANI/PMMA] // [Eu (BA) for aligning3phen/
PMMA] Janus nanobelt composition, the width of Janus nanobelt is 10.25 ± 0.3 μm, along Janus nanobelt length direction
Electric conductivity is strong, and conductance is 7.62 × 10-2S, and along, conductance 3.36 weak perpendicular to Janus nanobelt length direction electric conductivity
×10-10S, the two ratio are 2.27 × 108, there is strong anisotropic conductive, under the ultraviolet excitation of 290nm, lower layer
Film launches the bright red that main peak is located at 615nm；Mesopelagic layer is by unordered magnetic Fe3O4/ PVP composite nano fiber composition, directly
Diameter is 480 ± 3nm；Upper layer film is by unordered Tb (BA)3Phen/PAN composite nano fiber composition, diameter are 630 ± 5nm,
Under the ultraviolet excitation of 314nm, upper layer film launches the bright green light that main peak is located at 545nm；Prepared sandwich structure is multiple
The saturation magnetization for closing film is 5.14emu/g, has stronger magnetism；Prepared flexible sandwich structure composite membrane has
Good anisotropic conductive magnetism red and green color fluorescent multifunctional characteristic.
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