CN110423305A - Regulate and control Fe3O4The method of@PVP@PNIPAM magnetic photonic crystal nano chain interparticle distance - Google Patents
Regulate and control Fe3O4The method of@PVP@PNIPAM magnetic photonic crystal nano chain interparticle distance Download PDFInfo
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- CN110423305A CN110423305A CN201910740893.6A CN201910740893A CN110423305A CN 110423305 A CN110423305 A CN 110423305A CN 201910740893 A CN201910740893 A CN 201910740893A CN 110423305 A CN110423305 A CN 110423305A
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- 239000004038 photonic crystal Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 19
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 29
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000004584 polyacrylic acid Substances 0.000 claims abstract description 15
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 14
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000033228 biological regulation Effects 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 238000006116 polymerization reaction Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- XMLYCEVDHLAQEL-UHFFFAOYSA-N 2-hydroxy-2-methyl-1-phenylpropan-1-one Chemical compound CC(C)(O)C(=O)C1=CC=CC=C1 XMLYCEVDHLAQEL-UHFFFAOYSA-N 0.000 claims description 3
- 230000000977 initiatory effect Effects 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 229940056319 ferrosoferric oxide Drugs 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims 1
- 150000001408 amides Chemical class 0.000 claims 1
- 239000011260 aqueous acid Substances 0.000 claims 1
- 230000001276 controlling effect Effects 0.000 claims 1
- 239000003292 glue Substances 0.000 claims 1
- -1 polypropylene Polymers 0.000 claims 1
- 229920001155 polypropylene Polymers 0.000 claims 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 230000008859 change Effects 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 47
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 14
- 239000002245 particle Substances 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 7
- 239000010415 colloidal nanoparticle Substances 0.000 description 6
- 238000000399 optical microscopy Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 230000002349 favourable effect Effects 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- 239000003086 colorant Substances 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- YICILWNDMQTUIY-UHFFFAOYSA-N 2-methylidenepentanamide Chemical compound CCCC(=C)C(N)=O YICILWNDMQTUIY-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920003213 poly(N-isopropyl acrylamide) Polymers 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 238000012800 visualization Methods 0.000 description 2
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 1
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- 239000001263 FEMA 3042 Substances 0.000 description 1
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical class [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical class O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 235000011091 sodium acetates Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
- 229940033123 tannic acid Drugs 0.000 description 1
- 235000015523 tannic acid Nutrition 0.000 description 1
- 229920002258 tannic acid Polymers 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/24—Homopolymers or copolymers of amides or imides
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- C08L39/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions of derivatives of such polymers
- C08L39/04—Homopolymers or copolymers of monomers containing heterocyclic rings having nitrogen as ring member
- C08L39/06—Homopolymers or copolymers of N-vinyl-pyrrolidones
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- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0018—Diamagnetic or paramagnetic materials, i.e. materials with low susceptibility and no hysteresis
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
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- H01F1/0081—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity one dimensional, i.e. linear or dendritic nanostructures in a non-magnetic matrix, e.g. Fe-nanowires in a nanoporous membrane
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- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The present invention relates to be related to a kind of regulation Fe3O4Easy, the controllable method of@PVP PNIPAM photonic crystal nanometer chain interparticle distance, by adjusting the ratio between amount of polyacrylic acid concentration of aqueous solution or/and methylene diacrylamide and n-isopropyl acrylamide substance regulation Fe in reaction system3O4The interparticle distance of@PVP@PNIPAM magnetic photonic crystal nano chain, the polyacrylic acid concentration of aqueous solution change within the scope of 0.33~1.09g/L, and the ratio between methylene diacrylamide and the amount of n-isopropyl acrylamide substance change in 0.01~0.1 range.The present invention due to the adoption of the above technical solution, is allowed to compared with prior art, have the following advantages that and good effect: 1) its method is simple, efficient, at low cost, controllability and reproducible, is easy to industrial application popularization.2) its brightness and coloration modification scope are wide, and regulation method is simple, efficient.
Description
Technical field
The present invention relates to magnetic Nano material technical fields, and in particular to a kind of regulation Fe3O4@PVP@PNIPAM photon is brilliant
Easy, the controllable method of body nano chain interparticle distance.
Background technique
Compared to traditional inorganic pigment and organic dyestuff, schemochrome has environmentally friendly, energy saving, colour-fast, easy adjusting etc. excellent
Point has important potential application in the fields such as visualization sensing, display, anti-fake, camouflage, and magnetic photonic crystal is as a kind of important
Schemochrome material, because preparation method is simple, the speed of response is fast, response is concerned due to reversible the advantages that.It is fixed according to Prague
Rule, the schemochrome of One-dimensional magneto-photonic crystal nano chain is mainly determined by its particle size and interparticle distance, currently based on super suitable
Magnetic ferroferric oxide (Fe3O4) colloidal nanoparticles One-dimensional magneto-photonic crystal preparation and its color control obtained weight
Want progress.Document [Angew.Chem.Int.Ed., 2011,50,3747-3750] discloses a kind of silica (SiO2)
Coat superparamagnetism Fe3O4The nano chain of colloidal nanoparticles, under external magnetic field, gained Fe3O4@SiO2Nano chain is shown surely
Fixed schemochrome, change outer magnetic field direction, it can be achieved that the display of color and hide, with various sizes of Fe3O4Colloidal nanoparticles
To assemble primitive, the nano chain of three kinds of colors of red, green, blue can be prepared.Document [Nanoscale, 2017,9,3105-3113]
Disclose a kind of silica (SiO2) cladding superparamagnetism Fe3O4The nanometer rods of colloidal nanoparticles, the nanometer rods are in different magnetic
Based on the regulation to lattice defect under field intensity, the regulation to colour brightness is realized.Change external magnetic field strength in preparation process,
The nanometer rods with different interparticle distances can be prepared.Patent [104629232 A of CN] and document [Nano Lett., 2018,
DOI:10.1021/acs.nanolett.7b04218] disclose a kind of responsiveness magnetic photonic crystal chain, the photonic crystal nano
Rice chain realizes the dynamic of color, quick, reversible regulation based on volume change of the responsive gel layer under the stimulation of outfield.At present
The color control of magnetic photonic crystal nano chain mainly by adjust assembling cell sizes, external magnetic field strength and environmental stimulus come
Realize, these methods there are complex process, it is high to equipment and environmental requirement the disadvantages of, develop a kind of simple, efficient, controllable side
Method prepares different colours photonic crystal nanometer chain and is of great significance.
Summary of the invention
The technical problems to be solved by the present invention are: providing a kind of regulation Fe3O4@PVP@PNIPAM magnetic photonic crystal is received
The method of rice chain interparticle distance, this method are not necessarily to change the size of particle size and externally-applied magnetic field, have simple, efficient, cost
Low, controllability and it is reproducible the advantages that, to different colours Fe3O4The preparation of@PVP@PNIPAM magnetic photonic crystal nano chain has
It is significant.
The present invention solves its technical problem, and the following technical solution is employed: regulation Fe3O4@PVP@PNIPAM magnetism photon is brilliant
The method of body nano chain interparticle distance, includes following steps:
N-isopropyl acrylamide, methylene diacrylamide, 2- hydroxy-2-methyl propiophenone are dispersed four oxidations three by S1
In iron colloidal nanoparticle solution, ultrasonic mixing is uniform, forms pre-polymerization liquid；
S2 takes above-mentioned pre-polymerization liquid, and polyacrylic acid aqueous solution is added thereto, and ultrasonic mixing is uniform, after applying external magnetic field, into
Row uv-light polymerization is centrifugated product and with ethanol washing after reaction, finally by gained Fe3O4@PVP@
PNIPAM magnetic photonic crystal nano chain is scattered in water or ethyl alcohol；
Wherein by adjusting polyacrylic acid concentration of aqueous solution or/and methylene diacrylamide and N- isopropyl in reaction system
The ratio between amount of acrylamide substance regulates and controls Fe3O4The interparticle distance of@PVP@PNIPAM magnetic photonic crystal nano chain, described is poly-
Acrylic acid aqueous solution concentration changes within the scope of 0.33~1.09g/L, methylene diacrylamide and n-isopropyl acrylamide object
The ratio between amount of matter changes in 0.01~0.1 range.
According to the above scheme, Fe3O4@PVP@PNIPAM magnetic photonic crystal nano chain is dispersed in water, can be outer by changing
Portion magnetic field and temperature realize that its brightness and coloration are adjustable respectively.
Contain a large amount of carboxyls in polyacrylic acid of the invention, it can be with the poly- second of ferroferric oxide gel nanoparticle shell
Alkene pyrrolidone and n-isopropyl acrylamide form hydrogen bond, and it is different to influence particle periphery N- for the concentration of polyacrylic acid in reaction system
The concentration of propylacrylamide monomer, polyacrylic acid concentration is higher, and the monomer concentration of particle periphery is higher, is conducive to it in particle
Surrounding polymerize, and forms fine and close polymeric shell layer, and particle is completely embedded in gained nano chain, and chain spacing is smaller.Polyacrylic acid is dense
When spending lower, the monomer concentration of particle periphery is low, and the polymeric shell layer of formation is thin, and ferroferric oxide gel is received in gained nano chain
Steric hindrance repulsion is larger between rice corpuscles, and chain spacing is larger.The double propylacrylamide contents of crosslinking agent methene in reaction system
Gao Shi, after light initiation polymerization, the interparticle poly-N-isopropyl acrylamide polymer network structure of gained nano chain is fine and close, particle
Spacing is smaller.When the double propylacrylamide contents of crosslinking agent methene are low in reaction system, after light initiation polymerization, gained nano chain grain
Poly-N-isopropyl acrylamide polymer network structure between son is loose, and interparticle distance is larger.
The Fe of method preparation provided by the present invention3O4@PVP@PNIPAM magnetic photonic crystal nano chain, brightness and color
It is as follows to spend principle of adjustment and control:
Prepared nano chain is in natural torsion state, with the increase of external magnetic field, chain is gradually sent out in no externally-applied magnetic field
Raw rotation and stretching, extension orientation, periodically improve, diffraction peak intensity increases, diffraction with the increase of magnetic field strength along magnetic direction
Peak position does not change, and it is adjustable intuitively to show as brightness under same coloration.In addition, shell poly-N-isopropyl acrylamide has temperature
Quick property, when the environmental temperature is changed, nano chain interparticle distance changes, and coloration also accordingly changes.
The present invention due to the adoption of the above technical solution, is allowed to compared with prior art, have the following advantages that and accumulate
Pole effect:
1) do not change magnetic particle size and externally-applied magnetic field size, the magnetic photonic crystal nanometer of different colours can be obtained
Chain, method is simple, efficient, at low cost, controllability and reproducible, is easy to industrial application popularization.
2) gained Fe3O4@PVP@PNIPAM magnetic photonic crystal nano chain aqueous dispersions, brightness and coloration modification scope
Extensively, regulation method is simple, efficient, in fields such as display, visualization sensing, anti-fake, camouflages with important potential application.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 products therefrom of embodiment；
Fig. 2 is the optical microscopy light field figure of 1 products therefrom of embodiment；
Fig. 3 is the infrared spectrogram of 1 products therefrom of embodiment；
Fig. 4 is the hot weight curve of 1 products therefrom of embodiment；
Fig. 5 is the hysteresis loop figure of 1 products therefrom of embodiment；
Fig. 6 is spectrogram of 1 products therefrom of embodiment under different temperatures and magnetic field strength；
Fig. 7 is the microscope dark field figure under 1 products therefrom of embodiment at 4 deg. celsius different magnetic field intensity；
Fig. 8 is microscope dark field figure of 1 products therefrom of embodiment under 32 degrees Celsius of lower different magnetic field intensity；
Fig. 9 is microscope dark field figure of 1 products therefrom of embodiment under 38 degrees Celsius of lower different magnetic field intensity；
Figure 10 is the scanning electron microscope (SEM) photograph of 2 products therefrom of embodiment；
Figure 11 is the optical microscopy light field figure of 2 products therefrom of embodiment；
Figure 12 is the spectrogram of embodiment 2 and 3 products therefrom of embodiment under different magnetic field intensity；
Figure 13 is the Optical microscope dark field figure of 2 products therefrom of embodiment；
Figure 14 is the scanning electron microscope (SEM) photograph of 3 products therefrom of embodiment；
Figure 15 is the optical microscopy light field figure of 3 products therefrom of embodiment；
Figure 16 is the Optical microscope dark field figure of 3 products therefrom of embodiment；
Figure 17 is the scanning electron microscope (SEM) photograph of 4 products therefrom of embodiment；
Figure 18 is the optical microscopy light field figure of 4 products therefrom of embodiment；
Figure 19 is spectrogram of 4-6 products therefrom of embodiment under different magnetic field intensity；
Figure 20 is the Optical microscope dark field figure of 4 products therefrom of embodiment；
Figure 21 is the scanning electron microscope (SEM) photograph of 5 products therefrom of embodiment；
Figure 22 is the optical microscopy light field figure of 5 products therefrom of embodiment；
Figure 23 is the Optical microscope dark field figure of 5 products therefrom of embodiment；
Figure 24 is the scanning electron microscope (SEM) photograph of 6 products therefrom of embodiment；
Figure 25 is the optical microscopy light field figure of 6 products therefrom of embodiment；
Figure 26 is the Optical microscope dark field figure of 6 products therefrom of embodiment；
Figure 27 is the scanning electron microscope (SEM) photograph of 7 products therefrom of embodiment.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1:
(1) using the method in document (Adv.Mater.2014,26,1058-1064), preparation superparamagnetism four oxidation three
Iron colloidal nanoparticles, the specific steps are as follows:
0.13 mM of polyvinylpyrrolidone (PVP), 0.06 mM of tannic acid are added to and fill 30 milliliters of second two
In the beaker of alcohol, 80 degree of lower heating stirrings are completely dissolved for 15 minutes to PVP, and above-mentioned solution is cooled to room temperature, is added thereto
34 mMs of anhydrous sodium acetates are added after stirring 30 minutes in 2.6 mMs of Iron trichloride hexahydrates, stir after forty minutes that gained is molten
Liquid is transferred to 50 milliliters of ptfe autoclave liners, and liner is put into stainless steel kettle and is reacted 10 hours at 200 degree, cooling
Ethyl alcohol and hydromagnetic separating, washing are used afterwards, are finally dispersed product in spare in 20 milliliters of dehydrated alcohols.
(2) pre-polymerization liquid is prepared:
The ethanol solution of ferroferric oxide gel nanoparticle in 0.3 milliliter (1) is taken, is centrifugated, discards supernatant liquid, to
1 milliliter of ethylene glycol is wherein added, ultrasound makes particle be uniformly dispersed, weighs 0.3 gram of n-isopropyl acrylamide, 0.0204 respectively
Gram methylene diacrylamide (the ratio between amount of substance of methylene diacrylamide and n-isopropyl acrylamide is 0.05), 0.05 gram
2- hydroxy-2-methyl propiophenone, is added in above-mentioned solution, and ultrasonic mixing is uniform, forms pre-polymerization liquid.
(3)Fe3O4The preparation of@PVP@PNIPAM magnetic photonic crystal nano chain:
Take 200 microlitres of above-mentioned pre-polymerization liquid in 5 milliliters of small beakers, it is 0.54 gram per liter of (g/ that 2 milliliters of concentration are added thereto
L polyacrylic acid aqueous solution), ultrasonic mixing is uniform, and small beaker is placed in right above magnet, and adjusting magnetic field strength is 725 Gausses,
After induction 30 seconds, ultraviolet lamp is opened, 120 seconds, after reaction, centrifugation point are polymerize under the conditions of ultraviolet light and induced by magnetic field
From and with ethanol washing 3 times, finally product is dispersed in water.
The scanning electron microscope (SEM) photograph of products therefrom, light field microscope figure, infrared spectrogram, hot weight curve, hysteresis loop figure, no
Spectrogram and microscope dark field figure under synthermal and magnetic field is as shown in Fig. 1-9, from scanning electron microscope and light field microscope figure
Product is the 1-dimention nano chain of favorable dispersibility, and average chain length is 15.5 microns, can be deduced in product by infrared spectrogram containing poly-
Nitrogen isopropyl grade acrylamide, ferroso-ferric oxide, hydrogen bond know that content of organics is 34.37% in product by thermogravimetric analysis figure calculating,
The saturation magnetization of product known to hysteresis loop is 33.09emu/g, and gained nano chain is in 4 degree, 32 known to spectrogram
Degree, 38 degree of diffraction peak are respectively 592 nanometers, 536 nanometers, 488 nanometers, and diffraction peak intensity increases with the increase of magnetic field strength
Add.The gained nano chain known to microscope dark field figure is in golden yellow, green, blue, and color at 4 degree, 32 degree, 38 degree respectively
Brightness increases with the increase of applied field strengths.
Embodiment 2:
It is identical as 1 step of embodiment, but methylene diacrylamide is 0.0041 gram of (i.e. methylene diacrylamide in pre-polymerization liquid
With the ratio between the amount of n-isopropyl acrylamide substance for 0.01), final product disperses in ethanol.The scanning electron microscope of products therefrom
Figure, light field microscope figure, spectrogram and dark field microscope figure are as shown in Figure 10-13.It can by scanning electron microscope and light field microscope figure
Know that products therefrom is the nano chain of favorable dispersibility, the diffraction peak of gained nano chain is 647 nanometers known to spectrogram, diffraction
Peak intensity increases with the increase of magnetic field strength.It is 88 nanometers according to the chain spacing that Bragg equation calculates gained nano chain.By
Microscope figure knows gained photonic crystal chain for red.
Embodiment 3:
It is identical as 1 step of embodiment, but methylene diacrylamide is 0.041 gram of (i.e. methylene diacrylamide in pre-polymerization liquid
With the ratio between the amount of n-isopropyl acrylamide substance for 0.1), final product disperses in ethanol.The spectrogram of products therefrom is swept
Electron microscope, light field microscope figure and dark field microscope figure such as Figure 12 are retouched, shown in 14-16.The products therefrom known to shape appearance figure is point
The good nano chain of property is dissipated, the diffraction peak of gained nano chain is 560 nanometers known to spectrogram, and diffraction peak intensity is strong with magnetic field
The increase of degree and increase.It is 56 nanometers according to the chain spacing that Bragg equation calculates gained nano chain.Known by dark field microscope figure
Gained photonic crystal chain is green.
Embodiment 4:
It is identical as 1 step of embodiment, but methylene diacrylamide is 0.0082 gram of (i.e. methylene diacrylamide in pre-polymerization liquid
With the ratio between the amount of n-isopropyl acrylamide substance for 0.02), final product disperses in ethanol.The shape appearance figure of products therefrom,
Spectrogram and microscope figure are as shown in Figure 17-20.Products therefrom is the nano chain of favorable dispersibility known to shape appearance figure, by spectrum
The diffraction peak of gained nano chain is 607 nanometers known to figure, and diffraction peak intensity increases with the increase of magnetic field strength.According to Bradley
The chain spacing of nano chain obtained by lattice equation calculation is 73 nanometers.Gained photonic crystal chain is yellowish green known to dark field microscope figure
Color.
Embodiment 5:
It is identical as 4 step of embodiment, but polyacrylic acid concentration used is 0.33 gram per liter.The spectrogram of products therefrom is swept
Electron microscope, light field microscope figure and dark field microscope figure such as Figure 19 are retouched, shown in 21-23.By scanning electron microscope (SEM) photograph and light field microscope
Products therefrom known to figure is the nano chain of favorable dispersibility, and the diffraction peak of gained nano chain is 656 nanometers known to spectrogram,
Diffraction peak intensity increases with the increase of magnetic field strength.It is received according to the chain spacing that Bragg equation calculates gained nano chain for 91
Rice.Gained photonic crystal chain is red known to dark field microscope figure.
Embodiment 6:
It is identical as 4 step of embodiment, but polyacrylic acid concentration used is 1.09 gram per liters.The spectrogram of products therefrom is swept
Electron microscope, light field microscope figure and dark field microscope figure such as Figure 19 are retouched, shown in 24-26.The products therefrom known to shape appearance figure is point
The good nano chain of property is dissipated, chain spacing is smaller, and the diffraction peak of gained nano chain is 527 nanometers known to spectrogram, diffraction maximum
Intensity increases with the increase of magnetic field strength.It is 44 nanometers according to the chain spacing that Bragg equation calculates gained nano chain.By dark
Gained photonic crystal chain is blue-green known to the microscope figure of field.
Embodiment 7:
It is identical as 1 step of embodiment, but methylene diacrylamide is 0.0123 gram of (i.e. methylene diacrylamide in pre-polymerization liquid
With the ratio between the amount of n-isopropyl acrylamide substance for 0.03), polyacrylic acid concentration used is 0.73 gram per liter.Products therefrom
Scanning electron microscope (SEM) photograph is as shown in figure 27.The products therefrom known to shape appearance figure is the nano chain of favorable dispersibility, the nano chain chain spacing
It is smaller.
Claims (2)
1. regulating and controlling Fe3O4The method of@PVP@PNIPAM magnetic photonic crystal nano chain interparticle distance, includes following steps:
N-isopropyl acrylamide, methylene diacrylamide, 2- hydroxy-2-methyl propiophenone are dispersed ferroso-ferric oxide glue by S1
In body nano-particle solution, ultrasonic mixing is uniform, forms pre-polymerization liquid；
S2 takes above-mentioned pre-polymerization liquid, and polyacrylic acid aqueous solution is added thereto, and ultrasonic mixing is uniform, after applying external magnetic field, carries out purple
Outer light initiation polymerization is centrifugated product and with ethanol washing after reaction, finally by gained Fe3O4@PVP@PNIPAM magnetic
Property photonic crystal nanometer chain is scattered in water or ethyl alcohol；
Wherein by adjusting polyacrylic acid concentration of aqueous solution or/and methylene diacrylamide and N- isopropyl propylene in reaction system
The ratio between amount of amide material regulates and controls Fe3O4The interparticle distance of@PVP@PNIPAM magnetic photonic crystal nano chain, the polypropylene
Aqueous acid concentration changes within the scope of 0.33~1.09g/L, methylene diacrylamide and n-isopropyl acrylamide substance
The ratio between amount changes in 0.01~0.1 range.
2. regulation Fe according to claim 13O4The method of@PVP@PNIPAM magnetic photonic crystal nano chain interparticle distance,
It is characterized in that prepared Fe3O4@PVP@PNIPAM magnetic photonic crystal nano chain is dispersed in water, can be outer by changing
Portion magnetic field and temperature realize that its brightness and coloration are adjustable respectively.
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