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 PDF

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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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photonic crystal
crystal ball
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orientation
magneto discoloration
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CN106444099A (en
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马会茹
谈亚丽
官建国
刘云
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Wuhan University of Technology WUT
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    • GPHYSICS
    • G02OPTICS
    • G02FOPTICAL 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
    • G02F1/00Devices 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
    • G02F1/01Devices 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 
    • G02F1/09Devices 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F120/00Homopolymers 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
    • C08F120/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/04Acids; Metal salts or ammonium salts thereof
    • C08F120/06Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/46Polymerisation initiated by wave energy or particle radiation
    • C08F2/48Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers 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
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52Amides or imides
    • C08F220/54Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide

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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

Can magneto discoloration auto-orientation photonic crystal ball and preparation method thereof
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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