WO2014154148A1 - 色彩饱和度可调控光子晶体材料制备方法及其应用 - Google Patents
色彩饱和度可调控光子晶体材料制备方法及其应用 Download PDFInfo
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- WO2014154148A1 WO2014154148A1 PCT/CN2014/074147 CN2014074147W WO2014154148A1 WO 2014154148 A1 WO2014154148 A1 WO 2014154148A1 CN 2014074147 W CN2014074147 W CN 2014074147W WO 2014154148 A1 WO2014154148 A1 WO 2014154148A1
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
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- 239000012046 mixed solvent Substances 0.000 claims description 2
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 9
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- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
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- OQLZINXFSUDMHM-UHFFFAOYSA-N Acetamidine Chemical compound CC(N)=N OQLZINXFSUDMHM-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 244000241796 Christia obcordata Species 0.000 description 1
- 241000692870 Inachis io Species 0.000 description 1
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- YBQJKVOFUMFBDE-UHFFFAOYSA-N methyl 2-methylprop-2-enoate;prop-2-enoic acid;styrene Chemical compound OC(=O)C=C.COC(=O)C(C)=C.C=CC1=CC=CC=C1 YBQJKVOFUMFBDE-UHFFFAOYSA-N 0.000 description 1
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- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/08—Germanium
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/54—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/605—Products containing multiple oriented crystallites, e.g. columnar crystallites
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
-
- 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
- G02F2202/00—Materials and properties
- G02F2202/32—Photonic crystals
Definitions
- Color saturation can regulate photonic crystal material preparation method and application thereof
- the invention belongs to the field of materials and optics, and relates to a preparation method and application of a color saturation modulating photonic crystal material. Background technique
- Color is an indispensable element in the beautiful earth that constitutes human habitation. In our daily lives, colors are usually presented in the form of pigments, dyes, and pigments. The production of pigment dyes has led to the discharge of various waste water and waste gases, which have had a huge impact on the environment and have become one of the serious pollution sources in modern industry. Human beings are facing the most serious environmental crisis in history. Finding color materials with little or no pollution is becoming the consensus of all countries in the world today. scientistss have discovered in nature that some organisms such as butterfly wings and peacock feathers have a bright color that does not come from the role of pigments.
- Deep research has found that they all have a special micro-nano-fine structure that selectively reflects visible light at a specific wavelength to present a variety of rich colors, also known as structural colors.
- the structural color is caused by the Bragg scattering of light by nano-structures, and is environmentally friendly and aging-resistant as compared with pigments such as pigments and pigments, and is not easily faded over time.
- S. John and E. Yablonovitch have discovered that photoperiod band gaps in spatially periodic structures of different dielectric constant materials can control the behavior of light and propose the concept of photomc crystals.
- the use of photonic crystals to control the propagation of light to form structural colors has shown tremendous potential for development and market potential in the replacement of certain highly contaminated toxic dyes in applications such as coatings, cosmetics, fabrics, and displays.
- the method of preparing photonic crystals has both a "top-down” physical processing method and a “bottom-up” chemical assembly method.
- the nanoparticle self-assembly method can be nano-sized through the synthesis process because of its low cost, simple method, and no complicated equipment.
- the control of the morphology and structure of the particles realizes the preparation of photonic crystals with different functions.
- the color of the synthesized photonic crystal structure generally has problems such as white color of structure and low saturation of the hue, and some can only be observed from a specific angle direction to have obvious color, and there is a serious problem of viewing angle.
- the invention provides a preparation method and application of a color saturation modulatable photonic crystal material, comprising a photonic crystal of an opal structure and a preparation method of an opal structure photonic crystal and an application thereof.
- the present invention prepares a large-area, color-saturation-regulated photonic crystal material by preparing monodisperse microspheres in a container having a low adhesion force to water ⁇ ⁇ 500 ⁇ and a water contact angle CA of 90°.
- the present invention provides a method for preparing a color saturation modulatable photonic crystal material, the method comprising: mixing monodisperse microspheres with a solvent, adding a flux, and ultrasonically dispersing to form a uniform emulsion; In a container having a low adhesion (F) ⁇ 500 ⁇ for water and a contact angle (CA) of 90 to 90, at a temperature of 40 to 100 ° C and a humidity of 5% to 95%.
- F low adhesion
- CA contact angle
- the solvent is evaporated at the gas-liquid interface, causing the monodisperse microspheres in the emulsion to self-assemble at the gas-liquid interface to form an opal crystal photonic crystal material; wherein the monodisperse microspheres are monodisperse latex Granular or monodisperse silica microspheres; the feedstock is an aqueous light absorbing material, or carbon black particles, graphite, carbon nanotubes, fullerenes and derivatives thereof, graphene.
- the invention also provides a method for preparing an opal crystal of inverse opal structure, the method comprising: using the color saturation modulating photonic crystal material prepared by the above method as a sacrificial template, the gap between the monodisperse microspheres of the sacrificial template After filling the functional substance, the sacrificial mode is removed a photonic crystal having an inverse opal structure; wherein the functional substance is a sol of an inorganic oxide, a precursor for preparing a solid element, a polymer monomer or a polymer; and the inorganic oxide
- the sol is selected from the group consisting of a SiO 2 sol, a Ti 2 sol, a ZnO sol, and the like; the precursor for preparing a solid element is selected from the group consisting of: a precursor for preparing Si, a silicon precursor, a precursor for preparing C, or a Ge preparation.
- the precursor acetamidine; the polymer monomer is pyrrole; the polymer is an
- a photonic crystal material having a high saturation, large-area, high-quality opal structure can be formed; the photonic crystal material whose color saturation is controlled by the photonic crystal material has a good visual appearance effect;
- the invention relates to a method for preparing a color saturation modulating photonic crystal material, which is simple in operation, low in cost, green and environmentally friendly, and has good universality, and promotes photonic crystal as a printing material, a color display material, a decorative material, a personal cosmetic care material, and a fabric fiber.
- the practical application of materials, coating materials and anti-counterfeiting materials has important practical significance.
- Example 1 is an optical photograph of a photonic crystal material of high saturation color prepared by using monodisperse poly(styrene-methyl methacrylate-acrylic acid) latex particles in Example 1, which has a different viewing angle. Intense coloring.
- Fig. 2 is a scanning electron micrograph (magnification of 50,000 times) of a color saturation modulatable photonic crystal material prepared by using monodisperse poly(styrene-methyl methacrylate-acrylic acid) latex particles in Example 1. detailed description
- the method for preparing a color saturation modulating photonic crystal material comprises: mixing monodisperse microspheres with a solvent, adding a flux, and ultrasonically dispersing to form a uniform emulsion; and placing the obtained emulsion on the water with low adhesion Force (F) ⁇ 500 ⁇ , and the contact angle of water (CA) 90 is hydrophobic
- F adhesion Force
- CA contact angle of water
- the monodisperse microspheres are monodisperse latex particles or monodisperse silica microspheres
- the auxiliary material is an aqueous light absorbing material, and is carbon black particles, Graphite, carbon nanotubes, fullerenes and their derivatives, graphene or melanin.
- a series of photonic crystal materials having an adjustable saturation in the same color system can be realized.
- the obtained emulsion is placed on a hydrophobic substrate having a low adhesion (F) to water of 20 to 200 ⁇ M and a contact angle (CA) to water of 130 to 150°. Inside the container.
- F low adhesion
- CA contact angle
- the hydrophobic substrate having a low adhesion (F) ⁇ 500 ⁇ for water and a contact angle (CA) of 90 to water is a polymer substrate or covered with the polymer.
- the polymer is selected from the group consisting of polytetrafluoroethylene, polydimethylsiloxane, polyurethane, polyethylene, polyvinyl chloride and polystyrene; and the organic oil is liquid paraffin or silicone oil.
- the substrate covered with the polymer is, for example, a glass covered with polyurethane or the like.
- the monodisperse microspheres are monodisperse latex particles or monodisperse silica microspheres.
- the monodisperse latex particles are selected from the group consisting of monodisperse polystyrene latex particles, monodisperse polymethyl methacrylate latex particles, and monodisperse poly(styrene-methyl methacrylate-acrylic acid) polymer latex particles.
- monodisperse poly(styrene-methyl methacrylate-acrylic acid) polymer latex particles are monodisperse poly(styrene-methyl methacrylate-acrylic acid) polymer latex particles.
- the monodisperse microspheres may be known commercially available products having a particle size of 80 to 1100 nm. As such monodisperse microspheres, they can also be prepared by themselves (for example, refer to patent CN100381872C). Method for preparation).
- a monomer methyl methacrylate for example, a styrene monomer (for example, styrene and/or methyl styrene), a monomeric acrylic acid, a pH buffer (for example, ammonium hydrogencarbonate), and An emulsifier (for example, a mixture of sodium dodecylbenzenesulfonate and sodium dodecylsulfonate (weight ratio of 1:1)) according to methyl methacrylate: styrene monomer: acrylic acid: pH buffer : Emulsifier is 1: 19: 1 : 0.5: 0.0001 0.001 ratio (weight ratio) Dispersed in water to obtain a mixed system.
- a styrene monomer for example, styrene and/or methyl styrene
- a monomeric acrylic acid for example, a pH buffer (for example, ammonium hydrogencarbonate)
- An emulsifier for example, a mixture of sodium dode
- the monodisperse microspheres have a weight fraction in the emulsion of 0.01 to 90% by weight, preferably 0.01 to 30% by weight, more preferably 5 to 25% by weight, further preferably 10 to 20% by weight.
- the weight fraction of the auxiliary in the emulsion is from 0 to 10% by weight, preferably from 1 to 8% by weight, more preferably from 2 to 5% by weight; the others are solvents.
- the monodisperse microspheres have a weight fraction of 10 to 90% by weight in the emulsion, and the weight fraction of the auxiliary material in the emulsion is 0 to 10% by weight. It is a solvent.
- the solvent is selected from the group consisting of water, ethanol or a water-ethanol mixed solvent.
- the color saturation obtained by the preparation method of the present invention can regulate the photonic band gap of the photonic crystal material to be between 200 and 2600 nm.
- the color saturation modulating photonic crystal material is selected from the group consisting of polystyrene, polymethyl methacrylate, poly(styrene-methyl methacrylate-acrylic acid) and silica opal structure photonic crystals. kind.
- the invention also provides a method for preparing an opal crystal of inverse opal structure, the method comprising:
- the color saturation modulating photonic crystal material prepared by the above method is used as a sacrificial template, and after filling the functional substance in the gap between the monodisperse microspheres of the sacrificial template, the sacrificial template is removed to prepare an inverse opal structure.
- the functional substance is a sol of an inorganic oxide, a precursor for preparing a solid element, a polymer monomer or a polymer; and the sol of the inorganic oxide is selected from the group consisting of a SiO 2 sol, a precursor of a Ti0 2 sol, a ZnO sol or the like; the precursor for preparing a solid element is selected from the group consisting of: a precursor for preparing Si, a precursor of sucrose for preparing C, or a precursor for preparing Ge;
- the polymer monomer is pyrrole; the polymer is an epoxy resin or a phenolic resin.
- the method of filling the functional substance as a sacrificial template is selected from the group consisting of drop coating, dip coating, spin coating, electrochemical deposition, chemical vapor deposition and lift filling.
- the method of removing the sacrificial template is selected from one or more of calcination, organic solvent (e.g., toluene or tetrahydrofuran, etc.) dissolution and hydrofluoric acid dissolution methods.
- organic solvent e.g., toluene or tetrahydrofuran, etc.
- the above calcination temperature is preferably 160 to 600 °C.
- the functional substance is one of a sol of an inorganic oxide, a precursor for preparing a solid element, a polymer monomer or a polymer.
- the sol of the inorganic oxide is one selected from the group consisting of a SiO 2 sol, a Ti 2 sol, and a ⁇ sol.
- the precursor for preparing the solid element is selected from the group consisting of: a precursor for preparing Si, silicon sulfonium precursor, a precursor for preparing C, sucrose, a precursor for preparing Ge, and the like.
- the polymer monomer is pyrrole or the like.
- the polymer is an epoxy resin, a phenol resin or the like.
- the photonic crystal of the inverse opal structure obtained by the above method has a photonic band gap of between 150 and 2,500 nm.
- the photonic crystal of the inverse opal structure is an inorganic oxide, a solid element or a polymer, and the inorganic oxide is selected from one of SiO 2 , 110 2 and ZnO, etc.; the solid element is selected from the group consisting of Si, C and Ge One of the compounds; the polymer is selected from the group consisting of polypyrrole, epoxy resin, and phenolic resin.
- the present invention also provides the above-mentioned saturation color modulating photonic crystal material (ie, opal structure light)
- the sub-crystal material) and the photonic crystal of the above inverse opal structure are used as printing materials, color display materials, decorative materials, personal cosmetic care materials, woven fabric materials, coating materials, and anti-counterfeiting materials.
- Example 1
- the monodisperse poly(styrene-methyl methacrylate-acrylic acid) latex particles having a particle diameter of 190 nm are mixed with an ethanol solvent, and then uniformly mixed with the auxiliary material (carbon black nanoparticles), and ultrasonically dispersed to obtain an emulsion (wherein The content of the dispersed poly(styrene-methyl methacrylate-acrylic acid) latex particles is 20% by weight, the content of the auxiliary material is 2% by weight, and the balance is solvent), and the obtained emulsion is placed in a perfluorosilicone-modified In the ITO glass container (the contact glass surface has a contact angle with water of 150° and adhesion to water of 20 ⁇ ), at a temperature of 70 ° C and a humidity of 5%, the solvent is at the gas-liquid interface.
- the auxiliary material carbon black nanoparticles
- the monodisperse microspheres in the emulsion self-assemble at the gas-liquid interface and transfer to the surface of the glass substrate to form an opal structure photonic crystal material with different color saturation (photonic crystal material has a photonic band gap of 470 nm).
- photonic crystal material has a photonic band gap of 470 nm.
- a monodisperse polymer latex particle having a polydispersity index of less than or equal to 0.005 and a particle size range of 234 nm is finally obtained.
- the monodisperse poly(styrene-methyl methacrylate-acrylic acid) latex particles having a particle diameter of 234 nm are mixed with pure water, and then uniformly mixed with the auxiliary material (melanin), and ultrasonically dispersed to obtain an emulsion (wherein, monodisperse polymerization) (styrene-methyl methacrylate-acrylic acid)
- the content of the latex particles is 10% by weight
- the content of the auxiliary material is 4% by weight, and the balance is a solvent
- the obtained emulsion is placed in a container of a polyurethane hydrophobic sheet (with The contact angle of water is 100, the adhesion to water is 220 ⁇ ), the evaporation of solvent at the gas-liquid interface, the monodisperse microspheres in the emulsion are at a temperature of 80 ° C and a humidity of 5%.
- the liquid interface self-assembles, it is transferred to the surface of the fiber fabric to form an o
- the monodisperse poly(styrene-methyl methacrylate-acrylic acid) latex particles having a particle diameter of 250 nm are mixed with a pure water solvent, and then uniformly mixed with the auxiliary material (carbon nanotubes), and ultrasonically dispersed to obtain an emulsion (wherein The monodisperse poly(styrene-methyl methacrylate monoacrylic acid) latex particle content is 10% by weight, the content of the auxiliary material is 5% by weight, and the balance is solvent), and the obtained emulsion is placed in a polyethylene plate container.
- the monodisperse poly(styrene-methyl methacrylate-acrylic acid) latex particles having a particle diameter of 190 nm are mixed with pure water, and then uniformly mixed with the auxiliary material (carbon nanotubes), and ultrasonically dispersed to obtain an emulsion (wherein Disperse poly(styrene-methyl methacrylate-acrylic acid)
- the content of latex particles is 10% by weight, the content of the auxiliary material is 3% by weight, and the balance is solvent
- the obtained emulsion is placed in a container of polyethylene sheet (The contact angle of the surface with water is 130°, the adhesion to water is 100 ⁇ ), the evaporation of the solvent at the gas-liquid interface, the monodispersion in the emulsion at a temperature of 60 ° C and a humidity of 60%.
- the microspheres are self-assembled at the gas-liquid interface and deposited on the bottom of the container to form opals of different color saturation.
- the photonic crystal material photonic crystal material has a photonic band gap of 470 nm
- the opal structure photonic crystal material is ground into a fine particle powder, and further dispersed in pure water to obtain a photonic crystal ink material with different color saturation.
- the monodisperse poly(styrene-methyl methacrylate-acrylic acid) latex microspheres having a particle diameter of 217 nm are ultrasonically dispersed in water, uniformly mixed with the auxiliary material (carbon nanotubes), and ultrasonically dispersed to obtain an emulsion (the single Disperse poly(styrene-methyl methacrylate-acrylic acid)
- the content of latex particles is 10% by weight, the content of the auxiliary material is 2% by weight, and the balance is solvent.
- the obtained emulsion is placed in a container of polyethylene sheet.
- the contact angle of the surface with water is 130°, the adhesion to water is ⁇ ), the evaporation of the solvent at the gas-liquid interface, the monodispersion in the emulsion at a temperature of 60 ° C and a humidity of 60%.
- the microspheres are transferred to the surface of the polymer film to form an opal structure photonic crystal material with different color saturation (the photonic band gap of the photonic crystal material is 515 nm).
- the monodisperse poly(styrene-methyl methacrylate-acrylic acid) latex particles having a particle diameter of 310 nm are mixed with a pure water solvent, and then uniformly mixed with the auxiliary material (carbon nanotubes), and ultrasonically dispersed to obtain an emulsion (where Monodisperse poly(styrene-methyl methacrylate-acrylic acid)
- the content of the latex particles is 10% by weight, the content of the auxiliary material is 3% by weight, and the balance is solvent), and the obtained emulsion is placed in a container of polyethylene sheet Inside (surface contact angle with water is 130°, adhesion to water is ⁇ ), at a temperature of 60 ° C, humidity of 60%, due to evaporation of solvent at the gas-liquid interface, in the emulsion
- the monodisperse microspheres are self-assembled at the gas-liquid interface and deposited on the bottom of the container to form an opal-structured photonic crystal material (the photonic band gap
- a monodisperse polymer latex particle having a polydispersity index of less than or equal to 0.005 and a particle size range of 310 nm is finally obtained.
- the monodisperse poly(styrene-methyl methacrylate-acrylic acid) latex particles having a particle diameter of 310 nm are mixed with a pure water solvent, and then uniformly mixed with the auxiliary material (carbon nanotubes), and ultrasonically dispersed to obtain an emulsion (where Monodisperse poly(styrene-methyl methacrylate-acrylic acid)
- the content of the latex particles is 10% by weight, the content of the auxiliary material is 3% by weight, and the balance is solvent), and the obtained emulsion is placed in a container of polyethylene sheet Inside (surface contact angle with water is 130°, adhesion to water is ⁇ ), at a temperature of 60 ° C, humidity of 60%, due to evaporation of solvent at the gas-liquid interface, in the emulsion
- the monodisperse microspheres are self-assembled at the gas-liquid interface and deposited on the bottom of the container to form an opal-structured photonic crystal material (the photonic band gap
- the photonic crystal of the self-supporting high quality single crystal opal structure prepared above is used as a sacrificial template, and the ZnO sol is dripped onto the monodisperse poly(styrene-methacrylic acid).
- the ZnO sol is dripped onto the monodisperse poly(styrene-methacrylic acid).
- calcination is carried out at 450 ° C to remove the monodisperse poly(styrene-methyl methacrylate-acrylic acid) latex particles, and the photonic band gap is obtained at 530 nm.
- Photonic crystals of different saturation ZnO inverse opal structures are used as a sacrificial template, and the ZnO sol is dripped onto the monodisperse poly(styrene-methacrylic acid).
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Abstract
本发明提供一种色彩饱和度可调控光子晶体材料的制备方法，包括：将单分散微球与溶剂混合，加入助料，超声分散，形成均匀乳液；将所得到的乳液置于对水具有低粘附力（F）＜500μN，且对水的接触角（CA）≥ 90°的疏水性基材的容器内，在温度为40～100℃，湿度为5%～95%的条件下，利用溶剂在气液界面上蒸发，引起乳液中的单分散微球可在气液界面发生自组装，形成蛋白石结构的光子晶体材料。本发明还提供一种反蛋白石结构的光子晶体的制备方法，包括：将上述的制备方法所制备得到的色彩饱和度可调控光子晶体材料作为牺牲模板，在牺牲模板的单分散微球之间的间隙中填充功能性物质后，再去除所述的牺牲模板。
Description
色彩饱和度可调控光子晶体材料制备方法及其应用 技术领域
本发明属于材料及光学领域，涉及一种色彩饱和度可调控光子晶体材料 的制备方法及其应用。 背景技术
色彩是构成人类居住的美丽地球中不可缺少的元素。在我们的日常生活 中， 色彩通常是以颜料、 染料、 色素的形式呈现。 色素染料的生产带来了各 种废水废气的排放， 都对环境产生了巨大的影响， 已成为现代工业严重的污 染源之一。 人类正面临有史以来最严重的环境危机， 寻找环境污染小甚至无 污染的色彩材料已成为当今世界各国发展的共识。科学家在自然界中发现一 些生物体例如蝴蝶翅膀、 孔雀羽毛所具有的亮丽颜色并不来源于色素的作 用。 深层的研究发现它们都具有特殊的微纳精细结构， 可以选择性反射特定 波长的可见光， 从而呈现出各种丰富的颜色， 这也被称为结构色。 结构色是 纳米微结构对光的布拉格散射造成的， 与颜料色素等材料对可见光吸收成色 相比， 对环境友好， 耐老化性也更佳， 随着使用时间推移不易褪色等特点。 自 1987年 S. John和 E. Yablonovitch发现不同介电常数材料在空间周期性排 列的结构产生光子禁带带隙可以控制光的行为， 并提出光子晶体 (photomc crystals)的概念。 利用光子晶体控制光的传播形成结构颜色在替代某些高污 染有毒色素染料在涂料、 化妆品、 纤维织物、 显示器等领域的应用都显现出 具有巨大的发展空间和市场潜力。
制备光子晶体的方法既有 "自上而下"（top-down) 的物理加工方法， 也可以通过 "自下而上"（bottom-up) 的化学组装法。 纳米粒子自组装法由 于具有成本低、 方法简单、 不需要复杂的设备， 可以通过合成过程中对纳米
粒子的形态、 结构的控制实现不同功能的光子晶体制备等优点。 但目前人工 合成的光子晶体结构颜色普遍存在结构色彩泛白， 色相饱和度低等问题， 有 的甚至只能从特定的角度方向观察才有明显的色彩， 存在严重的可视角问 题。 与染料或颜料相比， 饱和度色彩上的差距极大的限制了自组装光子晶体 材料在涂料、 纺织品、 显示器以及化妆品等色彩显示领域的应用。 快速而又 简单制备具有高饱和度色彩的光子晶体， 已成为目前光子晶体结构色走向实 际应用迫切需要解决的技术难题。 发明内容
本发明提供一种色彩饱和度可调控光子晶体材料的制备方法及其应用， 包括蛋白石结构的光子晶体及反蛋白石结构光子晶体的制备方法及其应用。
本发明通过在对水具有低粘附力 σ<500μΝ) 且对水接触角 CA 90° 的容器内将单分散微球制备得到大面积、 色彩饱和度可调控的光子晶体材 料。
由此， 本发明提供一种色彩饱和度可调控光子晶体材料的制备方法， 该 方法包括： 将单分散微球与溶剂混合， 加入助料， 超声分散， 形成均匀乳液; 将所得到的乳液置于对水具有低粘附力（F ) <500μΝ，且对水的接触角（CA) 90 的疏水性基材的容器内， 在温度为 40〜100°C， 湿度为 5%〜95%的条 件下， 利用溶剂在气液界面上蒸发， 引起乳液中的单分散微球可在气液界面 发生自组装， 形成蛋白石结构的光子晶体材料； 其中， 所述的单分散微球是 单分散乳胶粒或单分散二氧化硅微球； 所述助料为水性吸光性材料， 或碳黑 颗粒、 石墨、 碳纳米管、 富勒烯及其衍生物、 石墨烯。
本发明还提供一种反蛋白石结构的光子晶体的制备方法， 该方法包括： 将上述方法制备得到的色彩饱和度可调控光子晶体材料作为牺牲模板，在牺 牲模板的单分散微球之间的间隙中填充功能性物质后， 再去除所述的牺牲模
板， 制备得到反蛋白石结构的光子晶体； 其中所述功能性物质为无机氧化物 的溶胶、 制备固体单质的前驱体、 聚合物单体或聚合物中的一种； 所述的无 机氧化物的溶胶选自 Si02溶胶、 Ti02溶胶和 ZnO溶胶等中的一种； 所述的 制备固体单质的前驱体选自： 制备 Si的前驱体乙硅垸、 制备 C的前驱体蔗 糖或制备 Ge的前驱体乙锗垸； 所述的聚合物单体为吡咯； 所述的聚合物为 环氧树脂或酚醛树脂。
根据本发明的方法， 能够形成饱和度色彩高， 大面积、 高质量的蛋白石 结构的光子晶体材料； 该光子晶体材料的色彩饱和度可调控的光子晶体材料 具有良好的视觉呈现效果； 并且， 本发明的色彩饱和度可调控的光子晶体材 料的制备方法操作简便、 成本低廉、 绿色环保、 普适性好， 对推动光子晶体 作为印刷材料， 色彩显示材料， 装饰材料， 个人化妆护理材料、 织物纤维材 料、 涂层材料、 防伪材料的实际应用具有重要现实意义。 附图说明
图 1为实施例 1中，利用单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸) 乳胶粒制备得到的高饱和色彩的光子晶体材料的光学照片，其在不同的观察 角度下均呈现有强烈色彩的着色。
图 2为实施例 1中，利用单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸) 乳胶粒制备得到的色彩饱和度可调控光子晶体材料的扫描电镜照片（放大倍 数为 5万倍）。 具体实施方式
本发明提供的色彩饱和度可调控光子晶体材料的制备方法包括：将单分 散微球与溶剂混合， 加入助料， 超声分散， 形成均匀乳液； 将所得到的乳液 置于对水具有低粘附力 （F ) <500μΝ， 且对水的接触角 （CA) 90 的疏水
性基材的容器内， 在温度为 40〜100°C， 湿度为 5%〜95%的条件下， 利用溶 剂在气液界面上蒸发， 引起乳液中的单分散微球可在气液界面发生自组装， 形成蛋白石结构的光子晶体材料； 其中， 所述的单分散微球是单分散乳胶粒 或单分散二氧化硅微球；所述助料为水性吸光性材料，且为碳黑颗粒、石墨、 碳纳米管、 富勒烯及其衍生物、 石墨烯或黑色素。
根据本发明， 通过控制所述助料的含量， 可实现同一色系内饱和度可调 的系列光子晶体材料。
根据本发明，优选的情况下，将所得到的乳液置于对水具有低粘附力（F ) 为 20-200μΝ， 且对水的接触角 （CA) 为 130-150°的疏水性基材的容器内。
根据本发明， 所述的对水具有低粘附力 （F ) <500μΝ， 且对水的接触 角 （CA) 90 的疏水性基材为高分子基材， 或者为用所述高分子覆盖的基 材， 或者是在全氟硅垸蒸气中放置过的对水具有粘附力 （F ) <500μΝ， 且 对水的接触角 （CA) 90 的基材（例如在全氟硅垸蒸气中放置过的 ΙΤΟ玻 璃等）， 或者是用有机油覆盖的基材 （如液体石蜡覆盖的玻璃， 硅油覆盖的 硅片等）。
所述的高分子选自聚四氟乙烯、 聚二甲基硅氧垸、 聚氨酯、 聚乙烯、 聚 氯乙烯和聚苯乙烯中的一种； 所述的有机油是液体石蜡或硅油。
用所述高分子覆盖的基材例如为聚氨酯覆盖的玻璃等。
所述的单分散微球是单分散乳胶粒或单分散二氧化硅微球。
所述的单分散乳胶粒选自单分散聚苯乙烯乳胶粒、单分散聚甲基丙烯酸 甲酯乳胶粒、 单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸）聚合物乳胶粒 中的一种。 优选为单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸）聚合物乳 胶粒。
所述的单分散微球可以为已知市售产品， 其粒径是 80〜1100nm。 作为 这样的单分散微球也可以自行制备（例如可以参考专利 CN100381872C中的
方法进行制备）。 具体地， 优选以下的方法： 将单体甲基丙烯酸甲酯、 苯乙 烯系单体（例如苯乙烯和 /或甲基苯乙烯）、 单体丙烯酸、 pH缓冲剂（例如为 碳酸氢铵）及乳化剂（例如为十二垸基苯磺酸钠与十二垸基磺酸钠的混合物 (重量比为 1 : 1 ) ) 按照甲基丙烯酸甲酯： 苯乙烯系单体： 丙烯酸： pH缓冲 剂： 乳化剂为 1 : 19: 1 :0.5:0.0001 0.001 的比例 （重量比） 分散在水中， 得到 混合体系。 然后， 在搅拌下， 将混合体加热到 50〜80°C。 接着加入过硫酸铵 水溶液使反应开始进行， 反应 3〜6小时后再加入适量过硫酸铵水溶液， 最 终得到单分散聚合物乳胶粒。当改变其中乳化剂十二垸基苯磺酸钠与十二垸 基磺酸钠的混合物的用量可得到不同粒径范围的单分散乳胶粒。
根据本发明， 所述的单分散微球在乳液中的重量分数为 0.01〜90 重量 %， 优选为 0.01〜30重量％， 更优选为 5~25重量％， 进一歩优选为 10~20 重量％； 所述助料在乳液中的重量分数为 0~10重量％， 优选为 1-8重量％， 更优选为 2-5重量％； 其它为溶剂。
根据本发明， 作为一种优选的实施方式， 所述的单分散微球在乳液中的 重量分数为 10〜90重量％， 所述助料在乳液中的重量分数为 0~10重量％， 其它为溶剂。
根据本发明， 所述溶剂选自水、 乙醇或水-乙醇混合溶剂。
根据本发明， 优选温度为 60〜80°C， 湿度为 5%〜60%的条件下， 利用 溶剂在气液界面上蒸发， 引起乳液中的单分散微球可在气液界面发生自组 装， 形成蛋白石结构的光子晶体材料。
通过本发明的制备方法得到的色彩饱和度可调控光子晶体材料的光子 带隙在 200〜2600nm之间。所述的色彩饱和度可调控的光子晶体材料选自聚 苯乙烯、 聚甲基丙烯酸甲酯、 聚 （苯乙烯一甲基丙烯酸甲酯一丙烯酸）和二 氧化硅蛋白石结构的光子晶体中的一种。
本发明还提供一种反蛋白石结构的光子晶体的制备方法， 该方法包括：
将上述方法制备得到的色彩饱和度可调控光子晶体材料作为牺牲模板，在牺 牲模板的单分散微球之间的间隙中填充功能性物质后， 再去除所述的牺牲模 板， 制备得到反蛋白石结构的光子晶体； 其中所述功能性物质为无机氧化物 的溶胶、 制备固体单质的前驱体、 聚合物单体或聚合物中的一种； 所述的无 机氧化物的溶胶选自 Si02溶胶、 Ti02溶胶和 ZnO溶胶等中的一种； 所述的 制备固体单质的前驱体选自： 制备 Si的前驱体乙硅垸、 制备 C的前驱体蔗 糖或制备 Ge的前驱体乙锗垸； 所述的聚合物单体为吡咯； 所述的聚合物为 环氧树脂或酚醛树脂。
根据本发明，在作为牺牲模板中填充功能性物质的方法选自滴涂、浸涂、 旋涂、 电化学沉积、 化学气相沉积及提拉填充法。
根据本发明， 所述的去除牺牲模板的方法选自煅烧、 有机溶剂 （如： 甲 苯或四氢呋喃等） 溶解及氢氟酸溶解方法中的一种或几种。
上述的煅烧温度优选是 160〜600 °C。
根据本发明， 所述的功能性物质是无机氧化物的溶胶、 制备固体单质的 前驱体、聚合物单体或聚合物中的一种。所述的无机氧化物的溶胶选自 Si02 溶胶、 Ti02溶胶和 ΖηΟ溶胶等中的一种。 所述的制备固体单质的前驱体选 自： 制备 Si的前驱体乙硅垸、制备 C的前驱体蔗糖和制备 Ge的前驱体乙锗 垸等。所述的聚合物单体是吡咯等。所述的聚合物是环氧树脂或酚醛树脂等。
根据本发明，通过上述方法得到反蛋白石结构的光子晶体的光子带隙在 150〜2500nm之间。
所述反蛋白石结构的光子晶体为无机氧化物、 固体单质或聚合物， 所述 无机氧化物选自 Si02、 1102和 ZnO等中的一种； 所述固体单质选自 Si、 C 和 Ge等中的一种； 所述聚合物选自聚吡咯、 环氧树脂和酚醛树脂等中的一 种。
本发明还提供上述饱和度色彩可调控光子晶体材料（即蛋白石结构的光
子晶体材料） 以及上述反蛋白石结构的光子晶体在作为印刷材料、 色彩显示 材料、 装饰材料、 个人化妆护理材料、 织物纤维材料、 涂层材料和防伪材料 中的应用。 实施例 1
将单体混合物甲基丙烯酸甲酯 (1.0 克)、 苯乙烯 (10 克)、 甲基苯乙烯 (9 克:)及丙烯酸 (1.0克：)， pH缓冲剂碳酸氢铵 (0.5克:)及乳化剂十二垸基苯磺酸钠 与十二垸基磺酸钠的混合物 (：重量比 1: 1， 重量为 12.29mg;>分散在水 (lOOmL) 中， 将所得到的混合体系在 500rpm搅拌混合， 并加热到 65°C。 加入 10毫 升的过硫酸铵0.5克溶解在 20毫升水中:)水溶液使反应开始进行， 反应 4.5 小时后再加入 5毫升的过硫酸铵水溶液， 其余的过硫酸铵水溶液在继续反应 4.5小时后加入， 反应随后持续 3小时结束。 最终得到多分散指数小于或等 于 0.005， 粒径范围为 190nm的单分散聚合物乳胶粒。
将粒径为 190nm 的单分散聚 （苯乙烯一甲基丙烯酸甲酯一丙烯酸） 乳 胶粒与乙醇溶剂混合后， 再与助料（碳黑纳米颗粒）均匀混合， 超声分散后 得到乳液（其中单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸）乳胶粒的含 量为 20重量％， 助料的含量为 2重量％， 余量为溶剂）， 将得到的乳液置于 全氟硅垸修饰的 ITO玻璃容器内 （修饰后的玻璃表面与水的接触角为 150°, 对水的粘附力为 20μΝ)， 在温度为 70°C、 湿度为 5%的条件下， 溶剂在气液 界面处的蒸发， 乳液中的单分散微球在气液界面发生自组装后， 转移到玻璃 基底表面， 形成不同色彩饱和度的蛋白石结构光子晶体材料（光子晶体材料 的光子带隙为 470nm)。 实施例 2
将单体混合物甲基丙烯酸甲酯 (1.0 克)、 苯乙烯 (10 克)、 甲基苯乙烯 (9
克:)及丙烯酸 (1.0克：)， pH缓冲剂碳酸氢铵 (0.5克:)及乳化剂十二垸基苯磺酸钠 与十二垸基磺酸钠的混合物 (：重量比 1 : 1， 重量为 9.12mg;>分散在水 (lOOmL) 中， 将所得到的混合体系在 500rpm搅拌混合， 并加热到 65°C。 加入 10毫 升的过硫酸铵0.5克溶解在 20毫升水中:)水溶液使反应开始进行， 反应 4.5 小时后再加入 5毫升的过硫酸铵水溶液， 其余的过硫酸铵水溶液在继续反应 4.5小时后加入， 反应随后持续 3小时结束。 最终得到多分散指数小于或等 于 0.005， 粒径范围为 234nm的单分散聚合物乳胶粒。
将粒径为 234nm的单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸）乳胶粒与 纯水混合后， 再与助料 （黑色素） 均匀混合， 超声分散后得到乳液 （其中， 单分散聚 （苯乙烯一甲基丙烯酸甲酯一丙烯酸） 乳胶粒的含量为 10重量％， 助料的含量为 4 重量％， 余量为溶剂）， 将得到的乳液置于聚氨酯疏水板材 的容器内（与水的接触角为 100， 对水的粘附力为 220μΝ)， 在温度为 80°C、 湿度为 5%的条件下， 溶剂在气液界面处的蒸发， 乳液中的单分散微球在气 液界面发生自组装后， 转移到纤维织物等表面， 形成不同色彩饱和度的蛋白 石结构光子晶体材料 （光子晶体材料的光子带隙为 574nm)。 实施例 3
将单体混合物甲基丙烯酸甲酯 (1.0克)、苯乙烯 10克)、甲基苯乙烯 (9克) 及丙烯酸 (1.0克)， pH缓冲剂碳酸氢铵 (0.5克：)及乳化剂十二垸基苯磺酸钠与 十二垸基磺酸钠的混合物 (：重量比 1 : 1， 重量为 5.69mg;>分散在水 (lOOmL)中， 将所得到的混合体系在 500rpm搅拌混合， 并加热到 65°C。 加入 10毫升的 过硫酸铵 (0.5克溶解在 20毫升水中)水溶液使反应开始进行， 反应 4.5小时 后再加入 5毫升的过硫酸铵水溶液， 其余的过硫酸铵水溶液在继续反应 4.5 小时后加入， 反应随后持续 3 小时结束。 最终得到多分散指数小于或等于 0.005， 粒径范围为 250nm的单分散聚合物乳胶粒。
将粒径为 250nm的单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸）乳胶 粒与纯水溶剂混合后， 再与助料（碳纳米管）均匀混合， 超声分散后得到乳 液（其中， 单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸）乳胶粒的含量为 10重量％， 助料的含量为 5重量％， 余量为溶剂）， 将得到的乳液置于聚乙 烯板材的容器内 （表面与水的接触角为 130°， 对水的粘附力为 100μΝ)， 在 温度为 60°C、 湿度为 60%的条件下， 溶剂在气液界面处的蒸发， 乳液中的 单分散微球在气液界面发生自组装后， 转移到聚合物薄膜表面， 形成不同色 彩饱和度的蛋白石结构光子晶体材料（光子晶体材料的光子带隙为 630nm)。 实施例 4
将单体混合物甲基丙烯酸甲酯 (1.0克)、苯乙烯 (10克)、甲基苯乙烯 (9克) 及丙烯酸 (1.0克)， pH缓冲剂碳酸氢铵 (0.5克：)及乳化剂十二垸基苯磺酸钠与 十二垸基磺酸钠的混合物 (：重量比 1 : 1，重量为 12.29mg;>分散在水 (lOOmL)中， 将所得到的混合体系在 500 rpm搅拌混合， 并加热到 65°C。 加入 10毫升的 过硫酸铵 (0.5克溶解在 20毫升水中)水溶液使反应开始进行， 反应 4.5小时 后再加入 5毫升的过硫酸铵水溶液， 其余的过硫酸铵水溶液在继续反应 4.5 小时后加入， 反应随后持续 3 小时结束。 最终得到多分散指数小于或等于 0.005， 粒径范围为 190nm的单分散聚合物乳胶粒。
将粒径为 190nm的单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸）乳胶 粒与纯水混合后，再与助料（碳纳米管）均匀混合，超声分散后得到乳液（其 中， 单分散聚 （苯乙烯一甲基丙烯酸甲酯一丙烯酸） 乳胶粒的含量为 10重 量％， 助料的含量为 3重量％， 余量为溶剂）， 将得到的乳液置于聚乙烯板材 的容器内 （表面与水的接触角为 130°， 对水的粘附力为 100μΝ)， 在温度为 60°C、 湿度为 60%的条件下， 溶剂在气液界面处的蒸发， 乳液中的单分散微 球在气液界面发生自组装后沉积在容器底部， 形成不同色彩饱和度的蛋白石
结构光子晶体材料 （光子晶体材料的光子带隙为 470nm)， 将该蛋白石结构 光子晶体材料研磨成微粒粉体， 进一歩分散在纯水内， 制得不同色彩饱和度 的光子晶体墨水材料。 实施例 5
将单体混合物甲基丙烯酸甲酯 (1.0 克)、 苯乙烯 (10 克)、 甲基苯乙烯 (9 克:)及丙烯酸 (1.0克：)， pH缓冲剂碳酸氢铵 (0.5克:)及乳化剂十二垸基苯磺酸钠 与十二垸基磺酸钠的混合物 (：重量比 1 : 1， 重量为 9.11mg;>分散在水 (lOOmL) 中， 将所得到的混合体系在 500rpm搅拌混合， 并加热到 65°C。 加入 10毫 升的过硫酸铵0.5克溶解在 20毫升水中:)水溶液使反应开始进行， 反应 4.5 小时后再加入 5毫升的过硫酸铵水溶液， 其余的过硫酸铵水溶液在继续反应 4.5小时后加入， 反应随后持续 3小时结束。 最终得到多分散指数小于或等 于 0.005， 粒径范围为 217nm的单分散聚合物乳胶粒。将粒径为 217nm的单 分散聚 （苯乙烯一甲基丙烯酸甲酯一丙烯酸） 乳胶粒微球超声分散于水中， 再与助料 （碳纳米管） 均匀混合， 超声分散后得到乳液（其中单分散聚 （苯 乙烯一甲基丙烯酸甲酯一丙烯酸） 乳胶粒的含量为 10 重量％， 助料的含量 为 2 重量％， 余量为溶剂）， 将得到的乳液置于聚乙烯板材的容器内 （表面 与水的接触角为 130°,对水的粘附力为 ΙΟΟμΝ) ,在温度为 60°C、湿度为 60% 的条件下， 溶剂在气液界面处的蒸发， 乳液中的单分散微球在气液界面发生 自组装后， 转移到聚合物薄膜表面， 形成不同色彩饱和度的蛋白石结构光子 晶体材料 （光子晶体材料的光子带隙为 515nm)。 实施例 6
将单体混合物甲基丙烯酸甲酯 (1.0 克)、 苯乙烯 (10 克)、 甲基苯乙烯 (9 克:)及丙烯酸 (1.0克：)， pH缓冲剂碳酸氢铵 (0.5克:)及乳化剂十二垸基苯磺酸钠
与十二垸基磺酸钠的混合物 (：重量比 1 : 1， 重量为 4.33mg;>分散在水 (lOOmL) 中， 将所得到的混合体系在 500 rpm搅拌混合， 并加热到 65°C。 加入 10毫 升的过硫酸铵0.5克溶解在 20毫升水中:)水溶液使反应开始进行， 反应 4.5 小时后再加入 5毫升的过硫酸铵水溶液， 其余的过硫酸铵水溶液在继续反应 4.5小时后加入， 反应随后持续 3小时结束。 最终得到多分散指数小于或等 于 0.005， 粒径范围为 310nm的单分散聚合物乳胶粒。
将粒径为 310nm 的单分散聚 （苯乙烯一甲基丙烯酸甲酯一丙烯酸） 乳 胶粒与纯水溶剂混合后， 再与助料 （碳纳米管）均匀混合， 超声分散后得到 乳液（其中， 单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸） 乳胶粒的含量 为 10重量％， 助料的含量为 3重量％， 余量为溶剂）， 将得到的乳液置于聚 乙烯板材的容器内 （表面与水的接触角为 130°， 对水的粘附力为 ΙΟΟμΝ) , 在温度为 60°C、 湿度为 60%的条件下， 由于溶剂在气液界面处的蒸发， 乳 液中的单分散微球在气液界面发生自组装后沉积在容器底部， 形成蛋白石结 构光子晶体材料 （光子晶体材料的光子带隙为 810nm)。 将上述制备得到的 蛋白石结构的光子晶体作为牺牲模板， 将含催化量的浓度为 98 重量％的浓 硫酸催化剂的 60 重量％蔗糖水溶液作为制备碳的前驱体， 用浸涂的方法填 充到构成所述牺牲模板的单分散聚甲基丙烯酸甲酯乳胶粒之间的间隙中，在 180°C下进行煅烧后， 并进一歩用甲苯溶解单分散聚甲基丙烯酸甲酯乳胶粒， 得到光子带隙位于 560nm的高饱和度的反蛋白石结构光子晶体。 实施例 7
将单体混合物甲基丙烯酸甲酯 (1.0 克)、 苯乙烯 (10 克)、 甲基苯乙烯 (9 克:)及丙烯酸 (1.0克：)， pH缓冲剂碳酸氢铵 (0.5克:)及乳化剂十二垸基苯磺酸钠 与十二垸基磺酸钠的混合物 (：重量比 1 : 1， 重量为 4.33mg;>分散在水 (lOOmL) 中， 将所得到的混合体系在 500rpm搅拌混合， 并加热到 65°C。 加入 10毫
升的过硫酸铵0.5克溶解在 20毫升水中:)水溶液使反应开始进行， 反应 4.5 小时后再加入 5毫升的过硫酸铵水溶液， 其余的过硫酸铵水溶液在继续反应 4.5小时后加入， 反应随后持续 3小时结束。 最终得到多分散指数小于或等 于 0.005， 粒径范围为 310nm的单分散聚合物乳胶粒。
将粒径为 310nm 的单分散聚 （苯乙烯一甲基丙烯酸甲酯一丙烯酸） 乳 胶粒与纯水溶剂混合后， 再与助料 （碳纳米管）均匀混合， 超声分散后得到 乳液（其中， 单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸） 乳胶粒的含量 为 10重量％， 助料的含量为 3重量％， 余量为溶剂）， 将得到的乳液置于聚 乙烯板材的容器内 （表面与水的接触角为 130°， 对水的粘附力为 ΙΟΟμΝ), 在温度为 60°C、 湿度为 60%的条件下， 由于溶剂在气液界面处的蒸发， 乳 液中的单分散微球在气液界面发生自组装后沉积在容器底部， 形成蛋白石结 构光子晶体材料 （光子晶体材料的光子带隙为 720nm)。 将上述制备得到的 蛋白石结构的光子晶体作为牺牲模板，将上述制备得到的自支撑高质量单晶 蛋白石结构的光子晶体作为牺牲模板， 将 ZnO溶胶滴涂到单分散聚 （苯乙 烯一甲基丙烯酸甲酯一丙烯酸）乳胶粒之间的间隙中，在 450°C下进行煅烧， 去除所述的单分散聚（苯乙烯一甲基丙烯酸甲酯一丙烯酸）乳胶粒， 可得到 光子带隙位于 530nm的不同饱和度 ZnO反蛋白石结构的光子晶体。
Claims
1、 一种色彩饱和度可调控光子晶体材料的制备方法， 其特征在于， 该 方法包括： 将单分散微球与溶剂混合， 加入助料， 超声分散， 形成均匀乳液; 将所得到的乳液置于对水具有低粘附力（F ) <500μΝ，且对水的接触角（CA) 90 的疏水性基材的容器内， 在温度为 40〜100°C， 湿度为 5%〜95%的条 件下， 利用溶剂在气液界面上蒸发， 引起乳液中的单分散微球可在气液界面 发生自组装， 形成蛋白石结构的光子晶体材料； 其中， 所述的单分散微球是 单分散乳胶粒或单分散二氧化硅微球； 所述助料为水性吸光性材料， 且为碳 黑颗粒、 石墨、 碳纳米管、 富勒烯及其衍生物、 石墨烯或黑色素。
2、 根据权利要求 1所述的制备方法， 其中， 所述对水具有粘附力 （F) <500μΝ， 且对水的接触角 （CA) ^90°的疏水性基材是高分子基材； 或者 是用高分子覆盖的基材； 或者是在全氟硅垸蒸气中放置过的对水具有粘附力
(F) <300μΝ， 且对水的接触角 （CA) 90 的基材； 或者是用有机油覆盖 的基材。
3、 根据权利要求 2所述的制备方法， 其中， 所述的高分子选自聚四氟 乙烯、 聚二甲基硅氧垸、 聚氨酯、 聚乙烯、 聚氯乙烯和聚苯乙烯中的一种； 所述的有机油是液体石蜡或硅油。
4、 根据权利要求 1所述的制备方法， 其中， 所述的单分散微球在乳液 中的重量分数为 0.01〜30重量％， 所述助料在乳液中的重量分数为 0~10重 量％， 其它为溶剂。
5、 根据权利要求 4所述的制备方法， 其中， 所述溶剂选自水、 乙醇或
水-乙醇混合溶剂。
6、 根据权利要求 1所述的制备方法， 其中， 所述的单分散微球的粒径 为 80〜1100nm; 所述的单分散微球可以是单分散乳胶粒或单分散二氧化硅 微球。
7、 根据权利要求 6所述的制备方法， 其中， 所述的单分散乳胶粒选自 单分散聚苯乙烯乳胶粒、 单分散聚甲基丙烯酸甲酯乳胶粒、 单分散聚（苯乙 烯一甲基丙烯酸甲酯一丙烯酸） 聚合物乳胶粒中的一种。
8、 根据权利要求 1所述的制备方法， 其中， 所述的蛋白石结构的光子 晶体的光子带隙在 200〜2600nm之间。
9、 一种反蛋白石结构的光子晶体的制备方法， 其特征在于， 该方法包 括： 将权利要求 1-8中任意一项所述的制备方法所制备得到的色彩饱和度可 调控光子晶体材料作为牺牲模板，在牺牲模板的单分散微球之间的间隙中填 充功能性物质后， 再去除所述的牺牲模板， 制备得到反蛋白石结构的光子晶 体； 其中， 所述功能性物质为无机氧化物的溶胶、 制备固体单质的前驱体、 聚合物单体或聚合物中的一种； 所述的无机氧化物的溶胶选自 Si02溶胶、
Ti02溶胶和 ZnO溶胶等中的一种； 所述的制备固体单质的前驱体选自： 制 备 Si的前驱体乙硅垸、制备 C的前驱体蔗糖或制备 Ge的前驱体乙锗垸； 所 述的聚合物单体为吡咯； 所述的聚合物为环氧树脂或酚醛树脂。
10、 根据权利要求 9所述的制备方法， 其中， 所述去除所述的牺牲模板 所采用的方法选自煅烧、 有机溶剂溶解及氢氟酸溶解方法中的一种或几种。
11、 根据权利要求 10所述的制备方法， 其中， 所述的煅烧温度是 160 。C〜600。C。
12、 根据权利要求 7或 8所述的制备方法， 其中， 所述反蛋白石结构的 光子晶体为无机氧化物、固体单质或聚合物；所述无机氧化物选自 Si02、 Ti02 和 ΖηΟ中的一种； 所述固体单质选自 Si、 C和 Ge中的一种； 所述聚合物选 自聚吡咯、 环氧树脂和酚醛树脂中的一种。
13、 根据权利要求 1所述的制备方法， 其中， 所述反蛋白石结构的光子 晶体的光子带隙在 150〜2500nm之间。
14、权利要求 1所述的方法制备的饱和度色彩可调控光子晶体材料或权 利要求 7制备反蛋白石结构的光子晶体在作为印刷材料， 色彩显示材料， 装 饰材料，个人化妆护理材料、织物纤维材料、涂层材料和防伪材料中的应用。
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