CN114164483B - Preparation method of microbubble-driven photonic pigment - Google Patents
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- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/08—Copolymers of styrene
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/18—Homopolymers or copolymers of nitriles
- C08J2333/20—Homopolymers or copolymers of acrylonitrile
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
Abstract
The invention relates to a preparation method of a microbubble-driven photon pigment, belonging to the field of materials. A method for preparing a microbubble-driven photonic pigment comprises preparing a color photonic crystal film on a flat substrate surface by using nanoparticles; immersing the obtained film and a substrate into acid or alkali solution with certain concentration, wherein the substrate reacts with the acid or alkali to generate micro bubbles, and folds and cracks are generated on the surface of the photonic crystal film; and then taking out the base material and the photonic crystal, putting the base material and the photonic crystal into water, and separating the photonic crystal from the base material to obtain dispersed colored micro-sheets, namely the photonic pigment. The method uses the impact force of micro bubbles formed between the substrate and the photonic crystal to fragment the photonic crystal structure color film assembled on the flat substrate and separate from the constraint of the substrate to form the structure color microchip.
Description
Technical Field
The invention relates to a preparation method of a microbubble-driven photon pigment, belonging to the field of materials.
Background
A photonic crystal is a periodic dielectric structure with photonic band gap characteristics that produce a color visible to the human eye when the photonic band gap falls in the visible region, i.e., a structural color. Compared with the pigment color, the photonic crystal structure color has higher color saturation and brightness, but the application of the structure color is limited by the substrate, because the highly ordered photonic crystal structure can be formed only on the flat substrate, thereby obtaining the bright structure color. Therefore, the structural color is not easy to be coated on a large scale like dye and pigment.
Disclosure of Invention
In order to solve the problem that the structural color can not be coated on a large scale, the invention provides a method for preparing micron-sized photonic crystal pigment.
The invention provides a method for preparing micron-sized photonic crystal pigment, which is characterized in that a photonic crystal structure color film assembled on a flat substrate is fragmented by utilizing the impact force of micro bubbles formed between the substrate and photonic crystals, and is separated from the constraint of the substrate to form structure color fragments. The method not only can give consideration to the structural color size and facilitate subsequent application, but also is beneficial to maintaining the structural order and the color saturation of the photonic crystal. Therefore, the prepared structural color microchip is expected to be used as a novel photon pigment.
A preparation method of a microbubble-driven photonic pigment comprises the steps of preparing a photonic crystal film on the surface of a flat substrate by using nanoparticles; immersing the obtained photonic crystal film and a base material into an acid or alkali solution with a certain concentration, and reacting the base material with the acid or alkali to generate micro bubbles so as to generate folds and cracks on the surface of the photonic crystal film; and then taking out the base material and the photonic crystal, putting the base material and the photonic crystal into water, and separating the photonic crystal from the base material to obtain dispersed colored fragments, namely the photonic pigment.
In the technical scheme, the photonic crystal film is prepared by the following method: alternately assembling two nano materials with different refractive indexes on a flat base material for 3-15 times by using a nano particle dispersion liquid, and heating the base material on a heating plate at 50-160 ℃ for 1-30 minutes after each assembly to obtain a multilayer photonic crystal film with bright color, wherein the size of the nano particles is 10-80 nm; the thickness of each layer of the photonic crystal is 40-200 nm; the assembling method is dip coating, spray coating or spin coating.
In the above technical scheme, the nanoparticle layer is assembled on the substrate by using a dip coating, spray coating or spin coating manner disclosed in the prior art. The material for preparing the photonic crystal thin film is required to be present in a solvent in the form of nanoparticles to form a uniform dispersing agent, and the solvent can be water, a water-alcohol mixed solution and the like.
In the above technical scheme, the flat base material is silicon, glass, quartz, zinc or iron base material. Preferably, the flat substrate is a silicon wafer, a glass sheet, a quartz sheet, a zinc sheet or an iron sheet.
In the above technical scheme, the acid is hydrochloric acid, phosphoric acid, acetic acid or hydrofluoric acid; the alkali is sodium hydroxide.
Further, the concentration of the acid solution is 1-15 wt.%, and the concentration of the alkali solution is 1-20 wt.%.
In the above technical solution, the nanoparticles include, but are not limited to, titanium oxide, zirconium oxide, tin oxide, silicon oxide, carbon black, polystyrene, polyacrylonitrile, poly (styrene-acrylic acid), poly (styrene-butyl acrylate), poly (methyl methacrylate-ethylene glycol dimethacrylate), poly (acrylamide-N, N' -methylenebisacrylamide), and polyurethane nanoparticles.
In the technical scheme, the selection of the acid or the alkali and the concentration of the acid or the alkali is related to the selection of the base material, and the selection is based on the fact that the acid or the alkali and the concentration of the base material can react and generate enough bubbles; meanwhile, the determination of the acid or the alkali and the concentration thereof is also related to the nano particles selected for the photonic crystal layer, preferably, the acid or the alkali does not react with the nano materials of the photonic crystal layer or the acid or the alkali generates weaker reaction, and the reaction does not influence the color characteristic of the photonic crystal.
In the above technical scheme, preferably, the photonic crystal film is placed in an acid with a concentration of 1-15 wt.% or an alkali solution with a concentration of 1-20 wt.%, and is soaked for 1-30 minutes, so that the base material reacts with the acid or the alkali to generate micro bubbles, gas escapes, and wrinkles and cracks are generated on the surface of the photonic crystal film.
In the technical scheme, the photonic crystal film is preferably taken out and put into water, the solution or the base material is disturbed or oscillated, and the base material is separated from the photonic crystal fragments; and taking out the substrate, dispersing the photonic crystal fragments in the solution to form a photonic pigment dispersion liquid with the size of 10-200 mu m, and removing the solution to obtain the photonic pigment.
The invention has the beneficial effects that: the invention provides a method for preparing micron-sized photonic crystal pigment, which utilizes the impact force of micro bubbles formed between a substrate and photonic crystals to fragment a photonic crystal structure color film assembled on a flat substrate and separate from the constraint of the substrate to form a structure color microchip. The method can not only give consideration to the structural color size and facilitate subsequent application, but also be beneficial to keeping the structural order and the color saturation of the photonic crystal. Therefore, the prepared structural color particles are expected to be used as a novel photon pigment.
Drawings
FIG. 1 is a scanning electron micrograph of a cross section of a photonic pigment obtained in step (3) of example 1.
FIG. 2 is a scanning electron micrograph of the photonic pigment obtained in step (3) of example 1.
FIG. 3 is a digital photograph (blue) of the aqueous dispersion of the photonic pigment obtained in step (3) of example 1.
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but will not limit the invention in any way.
The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
The specific implementation mode is as follows:
a method of preparing a microbubble driven photonic pigment, the method comprising the steps of:
(1) alternately assembling two nano materials with different refractive indexes on a flat base material for 3-15 times, placing the base material on a heating plate at 50-160 ℃ for heating for 1-30 minutes after each assembling is finished, and finally obtaining the photonic crystal film with bright color, wherein,
the size of the nano material is 10-80 nm; the thickness of each layer of the photonic crystal is 40-200 nm; the assembly method may be dip coating, spray coating or spin coating.
(2) And (3) putting the photonic crystal film into an acid or alkali solution with a certain concentration, and soaking for 1-30 minutes. The base material reacts with acid or alkali to generate bubbles, gas escapes, and a large number of fine cracks are formed on the surface of the photonic crystal film.
(3) And taking out the photonic crystal, putting the photonic crystal into water, disturbing the solution or oscillating the substrate, and separating the substrate from the photonic crystal fragments. Taking out the substrate, and dispersing the photonic crystal fragments in the solution to form a photonic pigment dispersion liquid with the size of 10-200 mu m.
(4) And removing the aqueous solution by filtration, evaporation and the like to obtain the photonic pigment.
The flat substrate may be a silicon, glass, quartz, zinc or iron substrate.
The acid can be dilute hydrochloric acid, dilute phosphoric acid, acetic acid or hydrofluoric acid; the base may be sodium hydroxide.
The material for preparing the photonic crystal thin film must exist in an aqueous solution or a water-alcohol mixed solution in the form of nanoparticles.
The nano material for preparing the photonic crystal can be an organic polymer, including polystyrene, polyacrylonitrile, poly (styrene-acrylic acid), poly (styrene-butyl acrylate), poly (methyl methacrylate-ethylene glycol dimethacrylate), poly (acrylamide-N, N' -methylenebisacrylamide), and polyurethane; and may also be inorganic and include titanium oxide, zirconium oxide, tin oxide, silicon oxide, or carbon black.
Example 1
(1) Poly (styrene-acrylic acid) having an average particle diameter of 55nm was dispersed with deionized water to a mass fraction of 2.4%.
Titanium oxide powder with an average particle size of 50nm was taken and dispersed in a mixed solution of water and ethanol at a volume ratio of 1:1 to obtain a titanium oxide dispersion liquid with a mass fraction of 2%.
And (3) alternately spin-coating the polymer and the titanium oxide on the quartz plate substrate, and respectively spin-coating for 3 times to obtain the photonic crystal film with bright color. At the end of each spin coating, the coating was heated on a hot plate at 80 ℃ for 5 minutes.
(2) And (3) putting the quartz plate base material assembled with the photonic crystal film into hydrofluoric acid solution with the mass fraction of 2%, soaking for 5 minutes to generate bubbles, and allowing gas to escape to form a large number of fine cracks on the surface of the photonic crystal film.
(3) And taking out the photonic crystal and the quartz substrate together, putting the photonic crystal and the quartz substrate into water, oscillating the substrate, and separating the substrate from photonic crystal fragments. And taking out the substrate, dispersing the photonic crystal fragments in the solution to form a photonic pigment dispersion liquid with the size of 10-200 mu m, filtering and drying to obtain the photonic pigment. FIG. 1 shows the microscopic cross-sectional morphology of the photonic pigment, which is seen to maintain a good multilayer structure; FIG. 2 shows the surface topography of a photonic pigment; FIG. 3 is a digital photograph of the dispersion, showing dispersed blue micro-slabs.
Example 2
The quartz substrate in step (1) of example 1 was replaced with a glass substrate, and the other steps were not changed.
Examples 3 to 7
The poly (styrene-acrylic acid) in step (1) of example 1 was replaced with polystyrene, polyacrylonitrile, poly (methyl methacrylate-ethylene glycol dimethacrylate), poly (acrylamide-N, N' -methylenebisacrylamide), polyurethane, and the other steps were unchanged.
Example 8
(1) Poly (styrene-acrylic acid) having an average particle diameter of 55nm was dispersed with deionized water to a mass fraction of 2.4%.
Titanium oxide powder with an average particle size of 50nm was taken and dispersed in a mixed solution of water and ethanol at a volume ratio of 1:1 to obtain a titanium oxide dispersion liquid with a mass fraction of 2%.
And (3) alternately spin-coating the polymer and the titanium oxide on the silicon substrate, and respectively spin-coating for 3 times to obtain the photonic crystal film with bright color. At the end of each spin coating, the coating was heated on a hot plate at 80 ℃ for 5 minutes.
(2) And (3) putting the silicon wafer assembled with the photonic crystal film into a sodium hydroxide solution with the mass fraction of 20%, soaking for 10 minutes, reacting to generate bubbles, and allowing gas to escape to form a large number of fine cracks on the surface of the photonic crystal film.
(3) Taking out the photonic crystal and the silicon wafer together, putting the photonic crystal and the silicon wafer into water, disturbing the solution or oscillating the silicon wafer, and separating the silicon wafer from the photonic crystal fragments. And taking out the silicon wafer, dispersing the photonic crystal fragments in the solution to form a photonic pigment dispersion liquid with the size of 10-200 mu m, filtering and drying to obtain the photonic pigment.
Examples 9 to 10
The silicon substrate in step (1) of example 8 was replaced with a zinc sheet and an iron sheet substrate, and the other steps were not changed.
Example 11
(1) Silicon oxide having an average particle diameter of 20nm was dispersed with deionized water to obtain a dispersion having a mass fraction of 10%.
Titanium oxide powder with an average particle size of 50nm was taken and dispersed in a mixed solution of water and ethanol at a volume ratio of 1:1 to obtain a titanium oxide dispersion liquid with a mass fraction of 2%.
And (3) alternately spin-coating silicon oxide and titanium oxide on the zinc sheet substrate, and respectively spin-coating for 3 times to obtain the photonic crystal film with bright color. At the end of each spin coating, the coating was heated on a hot plate at 100 ℃ for 5 minutes.
(2) And (3) putting the zinc sheet assembled with the photonic crystal film into a hydrochloric acid solution with the mass fraction of 4%, soaking for 10 minutes to generate bubbles, allowing gas to escape, and forming a large number of fine cracks on the surface of the photonic crystal film.
(3) And taking out the photonic crystal, putting the photonic crystal into water, disturbing the solution or oscillating the zinc sheet, and separating the zinc sheet from the photonic crystal fragments. And taking out the zinc sheet, dispersing the photonic crystal fragments in the solution to form a one-dimensional photonic pigment dispersion liquid with the size of 10-200 mu m, filtering and drying to obtain the photonic pigment.
Example 12
The zinc sheet substrate in the step (1) of example 11 was replaced with an iron sheet substrate, and the other steps were not changed.
Examples 13 to 14
The hydrochloric acid in step (2) of example 11 was changed to phosphoric acid or acetic acid, and the other steps were not changed.
Claims (7)
1. A preparation method of a microbubble-driven photonic pigment is characterized by comprising the following steps: preparing a color photonic crystal film on the surface of a flat substrate by using nano particles; immersing the obtained film and a substrate into acid or alkali solution with certain concentration, wherein the substrate reacts with the acid or alkali to generate micro bubbles, and folds and cracks are generated on the surface of the photonic crystal film; and then taking out the base material and the photonic crystal, putting the base material and the photonic crystal into water, and separating the photonic crystal from the base material to obtain dispersed colored micro-chips, namely the photonic pigment.
2. The method of claim 1, wherein: the photonic crystal film is prepared by the following method: alternately assembling two nano materials with different refractive indexes on a flat base material for 3-15 times by using a nano particle dispersion liquid, and after each assembling, placing the base material on a heating plate at 50-160 ℃ for heating for 1-30 minutes to obtain a multilayer photonic crystal film with bright color, wherein the size of the nano particles is 10-80 nm; the thickness of each layer of the photonic crystal is 40-200 nm; the assembly method is dip coating, spray coating or spin coating.
3. The method of claim 1, wherein: the flat base material is silicon, glass, quartz, zinc or iron base material.
4. The method of claim 1, wherein: the acid is hydrochloric acid, phosphoric acid, acetic acid or hydrofluoric acid; the alkali is sodium hydroxide.
5. The method of claim 1, wherein: the nano particles are titanium oxide, zirconium oxide, tin oxide, silicon oxide, carbon black, polystyrene, polyacrylonitrile, poly (styrene-acrylic acid), poly (styrene-butyl acrylate), poly (methyl methacrylate-ethylene glycol dimethacrylate), poly (acrylamide-N, N' -methylene bisacrylamide) or polyurethane nano particles.
6. The method of claim 1, wherein: the method comprises the steps of putting the photonic crystal film into 1-15 wt.% acid or 1-20 wt.% alkali solution, soaking for 1-30 minutes, enabling the base material to react with the acid or the alkali to generate micro bubbles, enabling gas to escape, and enabling the surface of the photonic crystal film to generate folds and cracks.
7. The method according to claim 1 or 2, characterized in that: taking out the photonic crystal film, putting the photonic crystal film into water, disturbing the solution or oscillating the base material, and separating the base material from the photonic crystal fragments; and taking out the substrate, dispersing the photonic crystal fragments in the solution to form a photonic pigment dispersion liquid with the size of 10-200 mu m, and filtering to obtain the photonic pigment microchip.
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