CN106444099B - Can magneto discoloration auto-orientation photonic crystal ball and preparation method thereof - Google Patents
Can magneto discoloration auto-orientation photonic crystal ball and preparation method thereof Download PDFInfo
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- CN106444099B CN106444099B CN201611184159.9A CN201611184159A CN106444099B CN 106444099 B CN106444099 B CN 106444099B CN 201611184159 A CN201611184159 A CN 201611184159A CN 106444099 B CN106444099 B CN 106444099B
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- 239000004038 photonic crystal Substances 0.000 title claims abstract description 54
- 238000002845 discoloration Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 239000011258 core-shell material Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000000084 colloidal system Substances 0.000 claims abstract description 9
- 239000011246 composite particle Substances 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- 238000006073 displacement reaction Methods 0.000 claims abstract description 7
- 239000000178 monomer Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 5
- -1 photoinitiator Substances 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 230000009471 action Effects 0.000 claims abstract description 3
- 239000011805 ball Substances 0.000 claims description 56
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
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- NIFQZIBYCXSINH-UHFFFAOYSA-N 2-methyl-2-morpholin-4-yl-1-(4-morpholin-4-ylphenyl)butan-1-one Chemical compound C=1C=C(N2CCOCC2)C=CC=1C(=O)C(C)(CC)N1CCOCC1 NIFQZIBYCXSINH-UHFFFAOYSA-N 0.000 claims description 2
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 2
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- 125000002252 acyl group Chemical group 0.000 claims description 2
- 229960002233 benzalkonium bromide Drugs 0.000 claims description 2
- KHSLHYAUZSPBIU-UHFFFAOYSA-M benzododecinium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 KHSLHYAUZSPBIU-UHFFFAOYSA-M 0.000 claims description 2
- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 claims description 2
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- 125000005442 diisocyanate group Chemical group 0.000 claims description 2
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- 125000005456 glyceride group Chemical group 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- YLHXLHGIAMFFBU-UHFFFAOYSA-N methyl phenylglyoxalate Chemical compound COC(=O)C(=O)C1=CC=CC=C1 YLHXLHGIAMFFBU-UHFFFAOYSA-N 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 claims description 2
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 claims description 2
- 229940113124 polysorbate 60 Drugs 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims 2
- 239000003292 glue Substances 0.000 claims 2
- 239000004593 Epoxy Substances 0.000 claims 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 claims 1
- HPAFOABSQZMTHE-UHFFFAOYSA-N phenyl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)C1=CC=CC=C1 HPAFOABSQZMTHE-UHFFFAOYSA-N 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims 1
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- 238000003860 storage Methods 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
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- 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
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- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
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- 229920001219 Polysorbate 40 Polymers 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229940040526 anhydrous sodium acetate Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 239000012769 display material Substances 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 229940056319 ferrosoferric oxide Drugs 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound 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
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- 238000012986 modification Methods 0.000 description 1
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- HZBAVWLZSLOCFR-UHFFFAOYSA-N oxosilane Chemical compound [SiH2]=O HZBAVWLZSLOCFR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 235000010483 polyoxyethylene sorbitan monopalmitate Nutrition 0.000 description 1
- 239000000249 polyoxyethylene sorbitan monopalmitate Substances 0.000 description 1
- 229940101027 polysorbate 40 Drugs 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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- 241000894007 species Species 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 150000003462 sulfoxides Chemical class 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
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- 239000001648 tannin Substances 0.000 description 1
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Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/09—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on magneto-optical elements, e.g. exhibiting Faraday effect
-
- 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
- C08F120/00—Homopolymers 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
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/04—Acids; Metal salts or ammonium salts thereof
- C08F120/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- 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
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Nonlinear Science (AREA)
- Power Engineering (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The present invention relates to it is a kind of can magneto discoloration auto-orientation photonic crystal ball and preparation method thereof, the pre-polymerization drop being made of monodispersed superparamagnetic nanometer crystal druse colloid Core-shell Composite Particles, polymerized monomer, crosslinking agent, photoinitiator, surfactant and dispersion liquid is entered in oily phase, drop solidifies under externally-applied magnetic field and action of ultraviolet light, gained photonic crystal ball is taken out after the reaction was completed, is washed and is carried out solvent displacement.Beneficial effects of the present invention: preparing and regulation method is simple, favorable repeatability;So that it is always maintained at solid-liquid structure, namely keep its can magneto discoloration auto-orientation performance;The mass center of photonic crystal ball is not overlapped with the centre of sphere, it is caused to be shown in the case where no externally-applied magnetic field acts on from colour developing feature, more energy efficient relative to classical magnetic field inducing color development from developing the color;Controllability is good.
Description
Technical field
The present invention relates to display material preparation field, more particularly to it is a kind of can magneto discoloration auto-orientation photonic crystal ball
And preparation method thereof.
Background technique
The photon crystal micro-ball being made of monodisperse particle generates beautiful due to the wherein periodic arrangement of monodisperse particle
Schemochrome.Particularly, by the 1-D photon crystal ball of superparamagnetic nanoparticle assembling because its is easy to assembly, brightness is high, band
Gap regulates and controls the extensive concern for the advantages that facilitating causing domestic and international researcher.Such as with four oxygen of superparamagnetic Silica-coated
The research for changing the 1-D photon crystal ball that three-iron core-shell particles are primitive achieves impressive progress.Such as document
[J.Am.Chem.Soc.2009, volume 131, page 15687] obtains that solid color is presented by emulsion polymerization one-step solidification
One-dimensional solid photonic crystal ball, the acquisition of other color photonic crystal balls can only be by changing externally-applied magnetic field during the preparation process
Magnetic field strength obtain.Document [Small, 2011, volume 9, page 1163] in microfluidic channel different parts by applying
The magnetic field one-step solidification of varying strength can be obtained present different colours one-dimensional solid photonic crystal ball, compared to the former, this
Preparation process more optimizes, and photonic crystal ball monodispersity obtained is good, size tunable.In addition, being with ferroso-ferric oxide particle
The research of the 1-D photon crystal ball of primitive also achieves impressive progress.As patent [utilizes micro-reaction device and externally-applied magnetic field system
The method of standby colour developing photon crystal micro-ball] these spherical drop shells are solidified using the method for uv photopolymerization, photonic crystal
The colour developing shell of structure is saved, and a period of time is placed, and prepared photon crystal micro-ball can be fully cured.This method is simple
Easy, the photonic crystal ball structure-controllable of preparation has important value to the preparation of magnetic field control photon crystal structure.These
Although 1-D photon crystal ball can show beautiful schemochrome under the influence of a magnetic field, and have magneto discoloration performance.But it is same
When there is also two aspect problems, first, the display of photonic crystal ball color depends on magnetic field;Second, its magneto discoloration performance by
Surrounding medium and magnetic direction are affected, poor controllability.
Summary of the invention
The technical problems to be solved by the present invention are: provide it is a kind of can magneto discoloration auto-orientation photonic crystal ball and its system
Preparation Method.Gained photonic crystal ball has auto-orientation colour developing and the performance characteristics along auto-orientation direction magneto discoloration, preparation method
Simply, favorable repeatability is of great significance to the preparation of magnetic field control photon crystal structure.
The present invention solves its technical problem, and the following technical solution is employed: it is a kind of can magneto discoloration auto-orientation photonic crystal
Ball is the asymmetric heterojunction structure of solid phase shell and liquid phase kernel, and the solid phase shell is by polymer substrate and fixation
It forms one-dimensional catenary structure by monodispersed superparamagnetic nanometer crystal druse colloid Core-shell Composite Particles in the polymer matrix to form, institute
The liquid phase kernel stated is made of monodispersed superparamagnetic nanometer crystal druse colloid Core-shell Composite Particles dispersion liquid, and the photon is brilliant
Body ball mass center is not overlapped with the centre of sphere.
It is described can magneto discoloration auto-orientation photonic crystal ball, unsymmetric structure refers to that solid phase shell thickness is uneven
Even, heterojunction structure, which refers to, has both solid-liquid two-phase, and the liquid phase kernel will not solidify during storage.
According to the above scheme, the polymer substrate is changed by one or more of organic matter containing acrylic acid groups
Learn the gel network being cross-linked into.
It is a kind of can magneto discoloration auto-orientation photonic crystal ball preparation method, it is characterised in that will be by monodispersed super suitable
What magnetic nanometer crystal druse colloid Core-shell Composite Particles, polymerized monomer, crosslinking agent, photoinitiator, surfactant and dispersion liquid formed
Pre-polymerization drop enters in oily phase, and drop solidifies under externally-applied magnetic field and action of ultraviolet light, takes out gained photonic crystal after the reaction was completed
Ball washs and carries out solvent displacement.
According to the above scheme, the polymerized monomer is one of organic matter containing acrylic acid groups or their group
It closes.
According to the above scheme, the crosslinking agent is N-N methylene-bisacrylamide, ethylene glycol dimethacrylate, ring
Oxosilane, poly- carbodiimide, methylene diacrylamide, diisocyanate.
According to the above scheme, the photoinitiator be 2- hydroxy-2-methyl -1- phenylacetone, diethoxy acetophenone, 2,
4,6- trimethylbenzoyl phenyl phosphonate esters, 1- hydroxycyclohexylphenylketone, 2- methyl -2- (4- morpholinyl) -1- [4- (4-
Morpholinyl) phenyl] -1- butanone, 2- hydroxy-2-methyl -1- phenyl -1- acetone, methyl benzoylformate, azodiisobutyronitrile,
Peroxidating two acyl or persulfate.
According to the above scheme, the surfactant be Triton X-100, alkaling earth metal base, benzalkonium bromide,
Fatty glyceride, polysorbas20, polysorbate40, polysorbate60, Tween 80, polysorbate85;The dispersion liquid is ethylene glycol, water, diformazan
Sulfoxide, dimethylformamide, acetic acid, alkanol, methylene chloride.
According to the above scheme, the viscosity of the oily phase is 3000cP~6000cP;A length of 250~the 400nm of ultraviolet light wave,
Curing time is 30~90s.
According to the above scheme, solvent displacement solvent for use is water, methanol, ethyl alcohol, dimethyl sulfoxide, dimethylformamide, tetrahydro
Furans or their mixture.
The present invention displaces uncured region except single point by control ultraviolet light curing time, and after the completion of preparation in time
Component other than scattered superparamagnetic nanometer crystal druse colloid Core-shell Composite Particles, obtained it is a kind of can magneto discoloration auto-orientation photon
Crystal ball.The photonic crystal ball is the liquid-solid asymmetric nuclear shell structure coexisted, including the photonic crystal shell that is cured and not by
Cured liquid core.For the photonic crystal ball in no externally-applied magnetic field, auto-orientation shows shell color;Apply magnetic along auto-orientation direction
When field, the chaining colour developing of nanoparticle orientation, shows kernel and shell dual-visualization and magneto discoloration characteristic in liquid core.These are special
Property not only assign photonic crystal ball more superior color developing, also make photonic crystal ball have more unique magneto discoloration
(change of its color can not only be realized energy by its deflection angle of flux control, moreover it is possible to not change its deflection angle
In the case of, it is realized only by the photon band gap for adjusting chain structure in liquid core.).With current gained 1-D photon crystal ball
It compares, the photonic crystal ball in the present invention has many advantages, such as simple preparation method, structure-controllable, from colour developing, Color tunable, aobvious
Show that the fields such as device, sensor, dc-dc converter and security devices have broad application prospects.
Beneficial effects of the present invention:
(1) microemulsion method and uv-light polymerization method is combined to prepare photonic crystal ball, preparation and regulation method it is simple,
Favorable repeatability.
(2) solvent replaces resulting photonic crystal ball, removes and removes monodispersed superparamagnetic nanometer crystal druse colloid core in liquid core
Component other than shell compound particle avoids the uncured region cured later of sphere, it is made to be always maintained at solid-liquid structure, namely
Keep its can magneto discoloration auto-orientation performance.
(3) mass center of photonic crystal ball is not overlapped with the centre of sphere, it is caused to show to develop the color certainly in the case where no externally-applied magnetic field acts on
Feature, it is more energy efficient relative to classical magnetic field inducing color development from developing the color.
(4) so that kernel nanoparticle is orientated chaining display color by applying outfield, and change colour not vulnerable to surrounding medium
And the influence of magnetic direction, controllability are good.
Detailed description of the invention
Fig. 1 is the field emission scanning electron microscope figure of products therefrom in embodiment 1.
Fig. 2~3 are digital photograph figure and field emission scanning electron microscope figure of the products therefrom when not adding magnetic field in embodiment 2.
Fig. 4 does not add digital photograph figure when magnetic field for products therefrom in embodiment 3.
Fig. 5 is the field emission scanning electron microscope figure of products therefrom in embodiment 4.
Fig. 6 is the digital photograph that products therefrom acquires under the effect of different magnetic field intensity along auto-orientation direction in embodiment 5
Figure.
Fig. 7 is the reflectance spectrum that products therefrom acquires under the effect of different magnetic field intensity along auto-orientation direction in embodiment 5
Figure.
Fig. 8 is the field emission scanning electron microscope image of products therefrom in embodiment 6.
Fig. 9 is the field emission scanning electron microscope image of products therefrom in embodiment 7.
Figure 10 (a)~(c) is the digital photograph figure of products therefrom in 8~embodiment of embodiment 10.
Figure 11 is the reflectance spectrum figure of products therefrom in 8~embodiment of embodiment 10.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated.It should be understood that these
Examples are only for illustrating the present invention and not for limiting the scope of the present invention.In addition, it should also be understood that, having read instruction of the present invention
Content after, those skilled in the art can make various modifications or changes to the present invention, and such equivalent forms equally fall within this
Apply for the appended claims limited range.
Embodiment 1
Tannic acid and polyvinylpyrrolidone are added in ethylene glycol and are configured to uniform mixed solution, tannin acid concentration is
3.33g/L, polyvinylpyrrolidoneconcentration concentration 400g/L.Then ferric chloride hexahydrate is added in mixed solution, is stirred to complete
Fully dissolved, the concentration 4.1g/L or 8.6g/L of ferric ion in solution.It is eventually adding anhydrous sodium acetate and adjusts pH to 9.0.So
After be put into reaction kettle, airtight heating to 200 DEG C, and keep the temperature 24 hours, be then cooled to room temperature, with ethyl alcohol clean separate 2~3
It is secondary, product is obtained after solids vacuum drying.As shown in figure 1 shown in the field emission scanning electron microscope image of the present embodiment product, institute
The product obtained is 150nm monodisperse colloid particle.
Embodiment 2
By 0.5g n-isopropyl acrylamide (NIPAM), 28.6mg N-N methylene-bisacrylamide (BIS), 22.8mg
2- hydroxy-2-methyl -1- phenylacetone (HMPP), 84.3mg Triton X-100 (Triton X-100) are added to
Ethylene glycol (EG) dispersion liquid of the resulting monodispersed superparamagnetic nanometer crystal druse colloid Core-shell Composite Particles of 5.0mg/mL embodiment 1
In, ultrasonic disperse is uniform, and it is spare to form pre-polymerization liquid.
It is 1mL with capacity, it is 5000cP oil phase that pre-polymerization liquid is added dropwise to and fills viscosity by the micro-syringe of syringe needle model 27G
Glassware in, at this time emulsion droplets in oily phase be in suspended state, stand half a minute after, by its as circular magnet just on
Side, regulating magnet and sample interval make magnetic field strength 260Gs, stand 30 seconds, and then opening power is 1000W, and wavelength is
365nm ultraviolet lamp is solidified, curing time 52s.Products therefrom is taken out after the reaction was completed and uses N,N-dimethylformamide
Washing, removes the oily phase of its surface remaining, is then washed with distilled water 3 times, and clean photonic crystal ball is transferred to and fills steaming
Solvent displacement is carried out in the centrifuge tube of distilled water, after 1 day, then is washed with distilled water 2 times, and product storage is standby in distilled water
With.Digital photograph of the products therefrom in the case where no externally-applied magnetic field acts on is as shown in Fig. 2, its display is uniform orange-yellow.By gained light
Sub- crystal ball is splitted along auto-orientation direction, is discarded core liquid and is freeze-dried, what gained section observed under scanning electron microscope
Pattern is as shown in figure 3, the magnetic particle that the photonic crystal spherical shell layer has asymmetry and shell includes is consolidated in the form of chain
Determine in the base.
Embodiment 3
It is identical as 2 step of embodiment, after the oil of photonic crystal ball surface mutually cleans up, clean photonic crystal ball is turned
Progress solvent displacement in the centrifuge tube for fill ethyl alcohol is moved to, after 1 day, then with ethanol washing 2 times, and in ethanol by product storage
It is spare.Digital photograph of the products therefrom under no externally-applied magnetic field is as shown in figure 4, its display is uniform orange red.It is retouched with embodiment 2
The Fig. 2 stated is the same, remains to that uniform schemochrome is presented in the case where getting rid of magnetic field.Illustrate the replacement for replacing solvent, not shadow
Ring the auto-orientation performance of photonic crystal ball.
Embodiment 4
Identical as 2 step of embodiment, monomer is 0.5g acrylic acid (AA).Monomer is acrylic acid and n-isopropyl acrylamide
When photonic crystal ball structure be consistent.As shown in figure 5, illustrate this method prepare the structure of resulting photonic crystal ball not by
The influence of monomeric species.
Embodiment 5
Products therefrom in above-described embodiment 2 is placed in distilled water, applies the magnetic field of varying strength along auto-orientation direction, adopts
Collect photonic crystal ball digital photograph figure as shown in Figure 6 and reflectance spectrum figure as shown in fig. 7, by digital photograph Fig. 6 it is found that with
The enhancing of magnetic field strength, the color that shell photon crystal structure is presented do not change, and liquid core nanoparticle is orientated chaining institute
Blue shift gradually occurs for the color of presentation, and color is successively rhodo, orange, dark green.By reflectance spectrum Fig. 7 it is found that with magnetic field strength
Enhancing, the reflection peak peak position of shell photon crystal structure do not move, and liquid core nanoparticle is orientated the reflection peak peak of chaining
Position gradually blue shift.
Embodiment 6
It is identical as 2 step of embodiment, but curing time is 30s.Gained photonic crystal ball is splitted along auto-orientation direction, is abandoned
It goes core liquid and is freeze-dried, the pattern that gained section observes under scanning electron microscope is as shown in figure 8, as seen from the figure, photon
The shell thickness of crystal ball is very thin, and long-time is placed easily rupturable in water.
Embodiment 7
It is identical as 2 step of embodiment, but curing time is 90s.Gained photonic crystal ball is splitted along auto-orientation direction, it is cold
Be lyophilized it is dry after, the pattern that gained section observes under scanning electron microscope is as shown in figure 9, as seen from the figure, photonic crystal ball is cured
Completely, become a solid sphere.
Embodiment 8
It is identical as 2 step of embodiment, but magnetic field strength is 600Gs.Products therefrom is placed in the digital photograph figure in distilled water
As shown in Figure 10 (a) and reflectance spectrum figure is as shown in figure 11, and the photonic crystal ball can be observed from digital photograph Figure 10 (a) and present
Bottle green, in conjunction with reflectance spectrum Figure 11 it is found that its reflection peak peak position is located at 535nm.
Embodiment 9
It is identical as 2 step of embodiment, but magnetic field strength is 330Gs.Products therefrom is placed in the digital photograph figure in distilled water
As shown in Figure 10 (b) and reflectance spectrum figure is as shown in figure 11, and the photonic crystal ball can be observed from digital photograph Figure 10 (b) and present
Yellow, in conjunction with reflectance spectrum Figure 11 it is found that its reflection peak peak position is located at 625nm.
Embodiment 10
It is identical as 2 step of embodiment, but magnetic field strength is 280Gs.Products therefrom is placed in the digital photograph figure in distilled water
As shown in Figure 10 (c) and emission spectrum is as shown in figure 11, the photonic crystal ball can be observed from digital photograph Figure 10 (c), tangerine is presented
Red, in conjunction with reflectance spectrum Figure 11 it is found that its reflection peak peak position is located at 670nm.
Claims (10)
1. one kind can magneto discoloration auto-orientation photonic crystal ball, be solid phase shell and liquid phase kernel asymmetric hetero-junctions
Structure, the solid phase shell are by polymer substrate and to fix in the polymer matrix by monodispersed superparamagnetic nanometer crystal druse glue
Body Core-shell Composite Particles form one-dimensional catenary structure composition, and the liquid phase kernel is by monodispersed superparamagnetic nanometer crystal druse glue
Body Core-shell Composite Particles dispersion liquid composition, the photonic crystal ball mass center are not overlapped with the centre of sphere.
2. it is according to claim 1 can magneto discoloration auto-orientation photonic crystal ball, it is characterised in that the polymer
Matrix is the gel network being chemically crosslinked by one or more of organic matter containing acrylic acid groups.
3. it is described in claim 1 can magneto discoloration auto-orientation photonic crystal ball preparation method, it is characterised in that will be by list
The superparamagnetic nanometer crystal druse colloid Core-shell Composite Particles of dispersion, polymerized monomer, crosslinking agent, photoinitiator, surfactant and point
The pre-polymerization drop of dispersion liquid composition enters in oily phase, and drop solidifies under externally-applied magnetic field and action of ultraviolet light, takes out institute after the reaction was completed
Photonic crystal ball is obtained, washs and carries out solvent displacement.
4. it is according to claim 3 can magneto discoloration auto-orientation photonic crystal ball preparation method, it is characterised in that institute
The polymerized monomer stated is one of organic matter containing acrylic acid groups or their combination.
5. it is according to claim 3 can magneto discoloration auto-orientation photonic crystal ball preparation method, it is characterised in that institute
The crosslinking agent stated is N-N methylene-bisacrylamide, ethylene glycol dimethacrylate, epoxy silane, poly- carbodiimide, methene
Bisacrylamide, diisocyanate.
6. it is according to claim 3 can magneto discoloration auto-orientation photonic crystal ball preparation method, it is characterised in that institute
The photoinitiator stated is 2- hydroxy-2-methyl -1- phenylacetone, diethoxy acetophenone, 2,4,6- trimethylbenzoyl benzene
Base phosphonate ester, 1- hydroxycyclohexylphenylketone, 2- methyl -2- (4- morpholinyl) -1- [4- (4- morpholinyl) phenyl] -1- butanone,
2- hydroxy-2-methyl -1- phenyl -1- acetone, methyl benzoylformate, azodiisobutyronitrile, peroxidating two acyl or persulfate.
7. it is according to claim 3 can magneto discoloration auto-orientation photonic crystal ball preparation method, it is characterised in that institute
The surfactant stated is Triton X-100, and alkaling earth metal base, benzalkonium bromide, fatty glyceride, polysorbas20 spits
Temperature 40, polysorbate60, Tween 80, polysorbate85;The dispersion liquid be ethylene glycol, water, dimethyl sulfoxide, dimethylformamide, acetic acid,
Alkanol, methylene chloride.
8. it is according to claim 3 can magneto discoloration auto-orientation photonic crystal ball preparation method, it is characterised in that institute
The viscosity for stating oily phase is 3000cP~6000cP;A length of 250~the 400nm of ultraviolet light wave, curing time are 30~90s.
9. it is according to claim 3 can magneto discoloration auto-orientation photonic crystal ball preparation method, it is characterised in that it is molten
Agent displacement solvent for use is water, methanol, ethyl alcohol, dimethyl sulfoxide, dimethylformamide, tetrahydrofuran or their mixture.
10. it is according to claim 3 can magneto discoloration auto-orientation photonic crystal ball preparation method, it is characterised in that institute
The adjustable range for the magnetic field strength stated is 200~700Gs.
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