CN104630876A - Method for preparing anisotropic photonic crystal - Google Patents
Method for preparing anisotropic photonic crystal Download PDFInfo
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- CN104630876A CN104630876A CN201510078784.4A CN201510078784A CN104630876A CN 104630876 A CN104630876 A CN 104630876A CN 201510078784 A CN201510078784 A CN 201510078784A CN 104630876 A CN104630876 A CN 104630876A
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Abstract
The invention discloses a method for preparing an anisotropic photonic crystal and relates to anisotropic photonic crystals. The method comprises the following steps: (1) adding a hydrophilic monomer, a hydrophobic monomer and a cross-linking agent into a solvent, introducing nitrogen, heating, carrying out a polymerization reaction, adding an initiator solution, further introducing nitrogen for reacting, thereby obtaining monodisperse special-shaped polymeric microspheres; and (2) dispersing the monodisperse special-shaped polymeric microspheres prepared in the step (1) into water, thus obtaining polymeric microsphere emulsion; putting a glass sheet into the polymeric microsphere emulsion, thereby obtaining the anisotropic photonic crystal after the moisture is completely volatilized. According to the addition of the cross-linking agent, cross-linking is performed inside a macromolecular chain, anisotropic microspheres of irregular shapes which are different from the previous microspheres are formed, the operating process is simple and feasible, and the obtained special-shaped microspheres are strictly monodisperse. The polymeric microspheres of special core-shell structures are prepared by polymerizing soap-free emulsion in one step, the operating process is simple and feasible, the produced polymeric microspheres do not contain any impurities such as a surfactant and a buffer agent, the product is pure, and the particle size is controllable.
Description
Technical field
The present invention relates to dimension Anisotropy Photonic Crystals, especially relate to a kind of preparation method of dimension Anisotropy Photonic Crystals.
Background technology
1987, Yab lonovit (Yablonovitch, E.1987.Phys.Rev.Lett.58,2059-2062.) and John (John, S.1987.Phys.Rev.Lett.58,2486-2489) propose the concept of photonic crystal (Photonic Crystal) respectively.Because photonic crystal has periodically adjustable specific inductivity, the light of propagation can be made to produce Bragg scattering, thus effectively can play the effect of optically focused and optical filtering, the physical phenomenons such as such as super prism, negative index can be produced, therefore cause the extensive concern of scientific circles.Photonic crystal, as the important advanced optical material of a class, has shown huge application prospect in photonic crystal reflection device, photon crystal filter, photodiode and photonic crystal fiber etc., becomes a kind of important materials building photonic device.The preparation technology of photonic crystal mainly contains the complicated semiconductor microactuator processing technology such as photoengraving, electrochemical etching, electron beam and focused-ion-beam lithography.Self-assembly method due to technique simple, and Van der Waals force, hydrogen bond, electrostatic force and surface tension etc. can realize the ordered arrangement of photonic crystal very well as its motivating force and be subject to extensive favor.
Dimension Anisotropy Photonic Crystals attracts wide attention due to its special structure properties, the symmetrical structure of rule bead causes the W point in polarization mode source region in cloth or the generation of U point to be with degeneracy, therefore for general medium ball, the full bandgap photonic crystal producing low refractive index is very difficult.And dimension Anisotropy Photonic Crystals is not owing to itself having symmetry, what assembled unit can effectively avoid symmetrical structure to cause can be with merger to make the preparation of the full bandgap photonic crystal of low refractive index become possibility, the structure that spheroidal particle can not be formed can be constructed, realize complete 3D or more tiny forbidden photon band, thus expand the application of photonic crystal.At present, dimension Anisotropy Photonic Crystals develops to some extent, as (Langmuir 2007 such as Ian D.Hosein and Chekesha M.Liddell, 23,8810-8814) prepare mushroom single dispersing PS polymer microballoon by suspension polymerization, and obtain the remote ordered structure of hexagon by convection current self-assembly, obtain the film that one deck is thin and transparent.Jin-Gyu Park (JACS2010,132,5960 – 5961) etc. produced (PS-co-TMSPA) polymkeric substance of dumbbell shaped by two-step approach seeded emulsion polymerization, and obtaining regularly arranged photon crystal structure by vertical hydatogenesis, the crystal film with photon obtained presents identical thickness and form in very large region.
In Chinese patent CN200510011219.2, the polyalcohol emulsion particle of hard core-soft core is utilized to prepare full-color colloid photonic crystal film, the method introduces hydrophilic, oleophylic monomer, in the course of the polymerization process hydrophilic monomer level off to water system formed shell, oleophylic monomer then trends towards the kernel that polymer spheres internal migration forms polymer microballoon, the microballoon that the effect formation rule of cooperative mechanical power is smooth, this method is a kind of by preparing regular microballoon and making its ordered arrangement produce the method for photonic crystal all the time, there is no the breakthrough of essence, cannot solution rule smooth ball formed photonic crystal can not the problem of long-living specific forbidden photon band.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of dimension Anisotropy Photonic Crystals.
Concrete steps of the present invention are as follows:
1) hydrophilic monomer, hydrophobic monomer, linking agent are added in solvent, carry out polyreaction after logical nitrogen heating, then add initiator solution, continue logical nitrogen reaction, obtain monodispersed profiled polymer microballoon;
2) by step 1) the single dispersing profiled polymer microballoon prepared is scattered in water, and obtain polymer microballoon emulsion, sheet glass is put into polymer microballoon emulsion, after moisture volatilizees completely, obtain dimension Anisotropy Photonic Crystals.
In step 1) in, described hydrophilic monomer, hydrophobic monomer, linking agent, solvent and initiator solution content by mass percentage can be: hydrophilic monomer and hydrophobic monomer are 1% ~ 20%, linking agent can be 2.5% ~ 25.4% of hydrophilic monomer and hydrophobic monomer total mass, initiator can be 0.1% ~ 5% of hydrophilic monomer and hydrophobic monomer total mass, and all the other are solvent; The volume ratio of described hydrophilic monomer and hydrophobic monomer can be 1: (3 ~ 20);
Described hydrophilic monomer can be selected from least one in glycidyl methacrylate, hydroxyethyl methylacrylate, NIPA, acrylamide, vinylformic acid etc.;
Described hydrophobic monomer can adopt vinylbenzene etc.;
Described linking agent can adopt Vinylstyrene etc.;
Described solvent can adopt water;
Described initiator solution can adopt Potassium Persulphate etc., and the mass percent concentration of initiator solution can be 0.2% ~ 2%.
The temperature of described heating can be 65 ~ 85 DEG C, and can stir during described polyreaction, stirring velocity can be 200 ~ 600rpm; The time that nitrogen reaction is led in described continuation can be 24h.
In step 2) in, the mass percentage concentration of described polymer microballoon emulsion can be 5% ~ 30%; Described sheet glass can use vitriolization in advance, and the time of process can be 12h; Sheet glass is preferably vertically put into polymer microballoon emulsion by described polymer microballoon emulsion of being put into by sheet glass, at 60 DEG C, along with the monodisperse polymer micro-sphere self-assembly in the evaporation emulsion of solvent, form the regular regular texture piled up, after moisture volatilizees completely, namely obtain the extensively adjustable dimension Anisotropy Photonic Crystals of color.
In the present invention, monodispersed heteromorphic nucleus shell structure polymer microballoon adopts the preparation of soap-free emulsion one-step synthesis, has that operation is simple, the homogeneous controlled advantage of products therefrom abnormity microspherulite diameter size.Owing to not adding any emulsifying agent and stablizer, products therefrom is pure, and follow-up polymer photon crystal of preparing does not need any process to use.The soap-free emulsion one-step polymerization method adopted, raw material is two kinds of monomers and the linking agent of hydrophilic and oleophylic, in the course of the polymerization process, hydrophilic segment trends towards aqueous solvent and forms shell, lipophilic ingredient then forms the kernel of polymer microballoon to polymer spheres internal migration, linking agent makes to be unified into one between macromole simultaneously, under the acting in conjunction of mechanical stirring power, forms monodispersed heteromorphic nucleus shell structure polymer microballoon.Its size can change the concentration of hydrophilic and oleophilic amount of monomer as required, changes initiator amount degree and change polymeric reaction temperature and stirring velocity and controls.
Special-shaped monodispersed core-shell structural polymer microballoon is adopted in the present invention, uniform emulsion is formed after in the water-soluble solvent of certain proportioning, the sheet glass of anticipating vertically is positioned in solution, and under certain temperature environment, along with the self-assembly of moisture evaporation profiled polymer microballoon forms the method for polymer photon crystal.The color of the photonic crystal obtained can regulate according to the difference of aeolosphere particle diameter; The concentration that the thickness of crystal film with photon depends on prepared profiled polymer microballoon emulsion and the amount of smearing.Due to the strict single dispersing of profiled polymer microballoon obtained, solution special-shaped ball in volatilization process is easy to stressed regularly arranged.Meanwhile, the special-shaped ball surface inclusion-free adopting emulsifier-free emulsion polymerization to obtain, is piling up the interference that can not be subject to impurity in alignment processes, is being conducive to the formation of ordered structure.
The present invention has broken tradition forms photonic crystal method with the regular bead arrangement of uniform particle diameter, has widened the generation field of polymer photon crystal.Meanwhile, define the forbidden photon band that regular smooth microballoon in the past can not be formed due to symmetrical, size reason, obtain narrower photon band gap, expand the range of application of photonic crystal.The profiled polymer photonic crystal obtained according to this method, due to its special structure and unique optical characteristics, has quite wide application prospect in Application Areass such as many finishing material, coating, film and solar concentrators; And pure in the present invention's strict single dispersing of special-shaped polymerizing microballoons used, require that strict field has unique advantage at environment-friendly materials, makeup etc.
The present invention prepares profiled polymer microballoon by emulsifier-free emulsion polymerization, a kind of anisotropic photonic crystal that utilized vertical deposition method to synthesize.The method introduces linking agent, in the course of the polymerization process hydrophilic monomer level off to water system formed shell, oleophylic monomer then trends towards the kernel that polymer spheres internal migration forms polymer microballoon, linking agent acts on monomer and realizes monomer interior polymeric, the effect that cooperative mechanical stirs, thus prepare and in the past different anisotropic polymer microballoons.And owing to adopting emulsifier-free emulsion polymerization, do not introduce any impurity as emulsifying agent, buffer reagent etc., the special-shaped microballoon obtained is pure, in self assembling process, the regularization arrangement of special-shaped microballoon is unaffected.The dimension Anisotropy Photonic Crystals prepared by this method can be formed in the past photonic crystal not getable more tiny photon band gap, greatly extend the application of photonic crystal.
The invention provides a kind of monodispersed heteromorphic nucleus shell structure method for preparing polymer micro.Especially the adding of linking agent, macromolecular chain inside is occurred crosslinked, define and in the past different anisotropy beads in irregular shape, its operating process simple possible, the strict single dispersing of special-shaped bead obtained.Due to special-shaped ball out-of-shape, do not possess the decay of the light wave hindering low photon band gap to be formed, after closely piling up can the smooth microballoon of formation rule due to symmetrical structure can not be formed photon band gap, the photon band gap obtained is narrower, thus expands the range of application of photonic crystal.Also widened the production field of photonic crystal, the smooth microballoon making the production of photonic crystal not only be confined to rule can also be obtained by the ordered arrangement of special-shaped microballoon simultaneously.Adopt the polymerization of soap-free emulsion single stage method to obtain the polymer microballoon of heteromorphic nucleus shell structure, its operating process is simple, and resulting polymer microballoon does not contain as the impurity such as tensio-active agent, buffer reagent, and products pure, size is controlled.Due to prepared profiled polymer microballoon and photonic crystal pure, extend its application at coating, dyestuff or pigment, film applications.
Accompanying drawing explanation
The SEM figure of the profiled polymer microballoon that Fig. 1 obtains for embodiment 1 and partial enlarged drawing.
The SEM figure of the profiled polymer microballoon that Fig. 2 obtains for embodiment 12 and partial enlarged drawing.
The SEM figure of the profiled polymer microballoon that Fig. 3 obtains for embodiment 13 and partial enlarged drawing.
The SEM figure of the profiled polymer microballoon that Fig. 4 obtains for embodiment 14 and partial enlarged drawing.
The SEM figure of the profiled polymer microballoon that Fig. 5 obtains for embodiment 2.
The SEM figure of the profiled polymer microballoon that Fig. 6 obtains for embodiment 5.
Fig. 7 is deposited on the photo that matrix obtains for the dimension Anisotropy Photonic Crystals that embodiment obtains.Wherein a, b, c, d, e figure is respectively embodiment 1 ~ 3, and 4 ~ 5,6,7 ~ 8,9 ~ 11.
Embodiment
The invention will be further described by reference to the accompanying drawings for embodiment below.
Embodiment 1:
By hydrophilic monomer glycidyl methacrylate 0.2mL, hydrophobic monomer vinylbenzene 2mL and Vinylstyrene 0.05mL adds logical nitrogen gas stirring 30 ~ 60min logical nitrogen continuously in the three-necked bottle containing 30mL deionized water, be warming up to 75 DEG C, then add the aqueous solution being dissolved with 0.04g Potassium Persulphate initiator.Reaction 24h, obtains the special-shaped copolymer microsphere emulsion of monodispersed styrene-divinylbenzene-glycidyl methacrylate (PS-DVB-PGMA).The SEM figure of profiled polymer microballoon and partial enlarged drawing are as shown in Figure 1.
At ambient pressure, microballoon obtained above is configured to dilute solution with the aqueous solution with 1:30 volume ratio and puts into this solution by vertical for the sheet glass soaking 12h with the vitriol oil, in the thermostatic drying chamber of 60 DEG C, place 24h.What produced by solution during evaporation makes the microballoon in solution Methodistic on the glass sheet arranged vertically to the surface tension effects of vertical glass sheet.Institute to obtain being deposited on matrix special-shaped photonic crystal as shown in a in Fig. 7.
Embodiment 2 ~ 11: with the processing condition of embodiment 1, change the add-on of water, the special-shaped copolymer microsphere emulsion of monodispersed styrene-divinylbenzene-glycidyl methacrylate (PS-DVB-PGMA) of synthesis different-grain diameter, the results are shown in Table 1.
Under room temperature, embodiment 2 ~ 11 gained monodispersed PS-DVB-PGMA profiled polymer microballoon emulsion water is mixed with the volume ratio of 1:30, and will vertically put into wherein with the sheet glass of vitriol oil immersion 12h in advance.Under the environment of normal pressure 60 DEG C, present the regular texture photonic crystal of unique color.What obtained to be deposited on matrix special-shaped photonic crystal as shown in b ~ e in Fig. 7.The SEM figure of the profiled polymer microballoon that embodiment 2 obtains is shown in Fig. 5, and the SEM figure of the profiled polymer microballoon that embodiment 5 obtains is shown in Fig. 6.
Table 1
With the processing condition of embodiment 1, change hydrophilic monomer is vinylformic acid, hydroxyethyl meth acrylate, acrylamide, the monodispersed styrene-divinylbenzene-vinylformic acid (PS-DVB-PAA) of synthesis heterogeneity, styrene-divinylbenzene-hydroxyethyl meth acrylate (PS-DVB-PHEMA), the special-shaped copolymer microsphere emulsion of styrene-divinylbenzene-acrylamide (PS-DVB-PAM).Obtain result as table 2.The SEM figure of profiled polymer microballoon and partial enlarged drawing are as shown in figs. 2 to 4.
Under room temperature, by monodispersed for embodiment 12 ~ 14 gained above-mentioned special-shaped microballoon with water with 1: 30 volume ratio mixing, and will vertically put into wherein with the sheet glass of vitriol oil immersion 12h in advance, under the environment of normal pressure 60 DEG C, after its moisture evaporation present the regular texture photonic crystal of unique color.
Table 2
The present invention adopts emulsifier-free emulsion polymerization method, prepares monodispersed heteromorphic nucleus shell structure polymer microballoon emulsion by adding linking agent.And this emulsion is mixed according to certain ratio with water, under normal pressure and certain temperature, the sheet glass of anticipating vertically is put into solution, with the volatilization of water solvent, special-shaped microballoon realizes self-assembly, is built into the polymer photon crystal of long-range order voluntarily.Formed crystal film with photon due to the structure of its uniqueness, excellent optical property, in Application Areass such as many finishing material, coating, film and solar concentrators, there is quite wide application prospect.
Claims (10)
1. a preparation method for dimension Anisotropy Photonic Crystals, is characterized in that its concrete steps are as follows:
1) hydrophilic monomer, hydrophobic monomer, linking agent are added in solvent, carry out polyreaction after logical nitrogen heating, then add initiator solution, continue logical nitrogen reaction, obtain monodispersed profiled polymer microballoon;
2) by step 1) the single dispersing profiled polymer microballoon prepared is scattered in water, and obtain polymer microballoon emulsion, sheet glass is put into polymer microballoon emulsion, after moisture volatilizees completely, obtain dimension Anisotropy Photonic Crystals.
2. the preparation method of a kind of dimension Anisotropy Photonic Crystals as claimed in claim 1, it is characterized in that in step 1) in, described hydrophilic monomer, hydrophobic monomer, linking agent, solvent and initiator solution content is by mass percentage: hydrophilic monomer and hydrophobic monomer are 1% ~ 20%, linking agent is 2.5% ~ 25.4% of hydrophilic monomer and hydrophobic monomer total mass, initiator is 0.1% ~ 5% of hydrophilic monomer and hydrophobic monomer total mass, and all the other are solvent; The volume ratio of described hydrophilic monomer and hydrophobic monomer is 1: (3 ~ 20).
3. the preparation method of a kind of dimension Anisotropy Photonic Crystals as claimed in claim 1, it is characterized in that in step 1) in, described hydrophilic monomer is selected from least one in glycidyl methacrylate, hydroxyethyl methylacrylate, NIPA, acrylamide, vinylformic acid.
4. the preparation method of a kind of dimension Anisotropy Photonic Crystals as claimed in claim 1, is characterized in that in step 1) in, described hydrophobic monomer adopts vinylbenzene.
5. the preparation method of a kind of dimension Anisotropy Photonic Crystals as claimed in claim 1, is characterized in that in step 1) in, described linking agent adopts Vinylstyrene.
6. the preparation method of a kind of dimension Anisotropy Photonic Crystals as claimed in claim 1, is characterized in that in step 1) in, described solvent adopts water.
7. the preparation method of a kind of dimension Anisotropy Photonic Crystals as claimed in claim 1, is characterized in that in step 1) in, described initiator solution adopts Potassium Persulphate, and the mass percent concentration of initiator solution can be 0.2% ~ 2%.
8. the preparation method of a kind of dimension Anisotropy Photonic Crystals as claimed in claim 1, is characterized in that in step 1) in, the temperature of described heating is 65 ~ 85 DEG C, stirs during described polyreaction, and stirring velocity is 200 ~ 600rpm; The time that nitrogen reaction is led in described continuation can be 24h.
9. the preparation method of a kind of dimension Anisotropy Photonic Crystals as claimed in claim 1, is characterized in that in step 2) in, the mass percentage concentration of described polymer microballoon emulsion is 5% ~ 30%.
10. the preparation method of a kind of dimension Anisotropy Photonic Crystals as claimed in claim 1, is characterized in that in step 2) in, described sheet glass uses vitriolization in advance, and the time of process is 12h; Sheet glass is preferably vertically put into polymer microballoon emulsion by described polymer microballoon emulsion of being put into by sheet glass, at 60 DEG C, along with the monodisperse polymer micro-sphere self-assembly in the evaporation emulsion of solvent, form the regular regular texture piled up, after moisture volatilizees completely, namely obtain the extensively adjustable dimension Anisotropy Photonic Crystals of color.
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| CN110305242A (en) * | 2019-07-02 | 2019-10-08 | 南京工业大学 | Preparation method of styrene-acrylic colloid emulsion with high solid content |
| CN112159492A (en) * | 2020-08-29 | 2021-01-01 | 浙江理工大学 | Heat-resistant photonic crystal element nano-microsphere and preparation method thereof |
| CN115594786A (en) * | 2022-11-10 | 2023-01-13 | 安徽工程大学（Cn） | P (St-co-GMA) -based structural yarn dyed fabric and macro rapid preparation method thereof |
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Application publication date: 20150520 |