CN112289871A - Laminated photonic crystal with optical performance regulation and control function and preparation method thereof - Google Patents
Laminated photonic crystal with optical performance regulation and control function and preparation method thereof Download PDFInfo
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0352—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions
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Abstract
The invention belongs to the field of optical materials and photochemistry, and discloses a laminated photonic crystal and a preparation method thereof. The laminated photonic crystal comprises a substrate, wherein a nano thin film layer is arranged on the substrate, a plurality of layers of unit photonic crystal thin film layers are arranged on the nano thin film layer, a nano thin film layer is also arranged between each layer of unit photonic crystal thin film layer, and the plurality of layers of unit photonic crystal thin film layers are formed by self-assembling colloidal microspheres with single microsphere size. The invention can realize optical regulation and control in the ultraviolet-visible-infrared full spectrum range, and has wide application potential in the fields of photocatalysis, optical display and control, micro-nano material synthesis and the like. The preparation method of the laminated photonic crystal disclosed by the invention is simple to operate, mild in condition, easy to regulate and control in optical performance and suitable for large-scale production.
Description
Technical Field
The invention belongs to the field of optical materials and photochemistry, and particularly relates to a laminated photonic crystal with optical performance regulation and control capability in an ultraviolet-visible-infrared full spectrum range and a preparation method thereof.
Background
Energy crisis and environmental pollution are two major problems in the sustainable development process of human beings. As is well known, sunlight has wide spectral range, high energy and environmental protection, and is the final source for maintaining the activities of various living bodies on the earth. The development of omnibearing and diversified utilization of light energy is the ultimate way to solve the problems of energy and environment. The photonic crystal is an ordered structure formed by periodically arranging two or more materials with different dielectric constants (refractive indexes), has unique optical characteristics of photon forbidden band, and the width and the position of the photon forbidden band can be modulated by the refractive index (or the dielectric constant) of a dielectric medium and the lattice parameter of the photonic crystal. Due to the existence of photon forbidden bands, the photonic crystal has outstanding advantages in regulating and controlling the propagation and motion states of light, which are different from those of general optical materials.
One of the common photonic crystal preparation methods expected to be developed in large scale at present is a colloidal microsphere self-assembly method. The method has the advantages of simple operation, easy assembly on a substrate and the like, but because the adhesion between colloid particles and the substrate is weak, the surface roughness is influenced by the size of the colloid particles, and the particles are influenced by the action of gravity, the obtained photonic crystal film is often thin, has more defects and is easy to fall off, so that the laminated photonic crystal is difficult to obtain. The scientific community has attempted to use O on the surface of a single-layer photonic crystal2The preparation of the laminated photonic crystal can be improved to a certain extent by processing with a method of plasma, ultraviolet lamp irradiation and loading of a layer of disordered template balls, and the laminated photonic crystal with 2-3 layers is obtained, but the research of preparing the laminated photonic crystal with multilayer stacking (more than 3 layers) is not reported so far, and the application of the photonic crystal is greatly limited.
Disclosure of Invention
The invention overcomes the defects of the prior art, and solves the technical problems that: the laminated photonic crystal film has the advantages that the number of layers which can be superposed is not limited in principle, the optical performance formed by superposing photon forbidden bands of unit photonic crystal film layers is realized, and the optical performance regulation in an ultraviolet-visible-infrared full spectrum range can be realized.
In order to solve the technical problems, the invention adopts the technical scheme that: the laminated photonic crystal with the optical performance regulation function comprises a substrate, wherein a nano thin film layer is arranged on the substrate, a plurality of layers of unit photonic crystal thin film layers are arranged on the nano thin film layer, a nano thin film layer is also arranged between every two layers of unit photonic crystal thin film layers, and the plurality of layers of unit photonic crystal thin film layers are formed by self-assembly of colloidal microspheres with single microsphere size.
The number of the unit photonic crystal thin film layers is 2-4; the nano film layers are made of one of silicon dioxide, titanium dioxide, tungsten trioxide, vanadium pentoxide, zinc oxide, tin dioxide, cadmium sulfide, zinc sulfide, copper sulfide, bismuth vanadate, bismuth tungstate, strontium titanate, sodium tantalate, BiOBr, g-C3N4, polystyrene, polymethyl acrylate and polyacrylamide, the thickness of the nano film layers arranged on the substrate is 2-5nm, and the thickness of the nano film layers between the unit photonic crystal film layers is 1-3 nm.
The invention also provides a preparation method of the laminated photonic crystal with optical performance regulation, which is characterized in that a monodisperse colloidal microsphere is utilized to carry out self-assembly on a substrate subjected to nano-level pretreatment to prepare a unit photonic crystal thin film layer; and then carrying out nano leveling pretreatment on the unit photonic crystal thin film layer, then carrying out self-assembly by using the monodisperse colloidal microspheres again, and carrying out the nano leveling pretreatment and the self-assembly of the monodisperse colloidal microspheres for multiple times in a circulating manner to form a laminated photonic crystal film formed by stacking multiple layers of unit photonic crystal thin films layer by layer, wherein each layer of unit photonic crystal thin film is formed by self-assembly of colloidal microspheres with single size.
The preparation method of the laminated photonic crystal with optical performance regulation and control comprises the following steps:
s1, soaking and cleaning the container and the substrate containing the colloidal microsphere solution, and then washing the container and the substrate clean by distilled water for later use;
s2, dissolving monodisperse colloidal microspheres with single microsphere size in a solvent, fully stirring and dispersing to prepare 0.02-3wt% colloidal microsphere solution for later use;
s3, performing nano-grade pretreatment on the cleaned substrate;
s4, inserting the pretreated substrate into the colloidal microsphere solution, placing the solution in a constant temperature and humidity environment, and self-assembling the solution on the substrate to form a unit photonic crystal thin film layer with a single microsphere size;
s5, replacing monodisperse colloid microsphere solutions with different sizes and concentrations, and repeating the steps S2-S4 for multiple times to obtain the laminated photonic crystal film.
In the step S3, the nano-planarization pretreatment method includes spin-coating, spray-coating, or pull-coating a nano-film, where the nano-film includes a metal compound and a polymer, and the metal compound is one of silicon dioxide, titanium dioxide, tungsten trioxide, vanadium pentoxide, zinc oxide, tin dioxide, cadmium sulfide, zinc sulfide, copper sulfide, bismuth vanadate, bismuth tungstate, strontium titanate, sodium tantalate, BiOBr, g-C3N4, polystyrene, polymethyl acrylate, and polyacrylamide.
In the step S2, the monodisperse colloidal microspheres are one of polymethyl methacrylate (PMMA), Polystyrene (PS), styrene-butyl acrylate-acrylic acid (PS-BA-AA) copolymer, Polyacrylamide (PAM), and silica; the solvent is water.
In the step S4, the corresponding parameters of the constant temperature and humidity environment are the temperature of 20-85 ℃ and the humidity of 30-90% RH.
In step S4, a single microsphere-sized unit photonic crystal film is formed on the substrate by self-assembly through vertical deposition, flow control deposition or a dip coating method.
The substrate is one of plane glass, curved glass, quartz, silicon wafers, metal, ceramic, polymer, fabric and flexible materials.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a laminated photonic crystal film and a preparation method thereof, which are characterized in that a laminated photonic crystal structure comprising a multilayer unit photonic crystal film is obtained by multilayer assembly of colloidal particles with different sizes after nano modification is carried out on a substrate and a bottom layer unit photonic crystal film, so that absorption and reflection of light with different wavelengths are realized, meanwhile, the absorption of light with different wavelengths can be regulated and controlled, and the laminated photonic crystal film has wide application potential in the aspects of photoelectrocatalysis, solar water decomposition, bionic materials, anti-counterfeiting marks, solar cells and the like. The method is simple to operate, short in time consumption, and capable of controlling the number of layers, and the prepared laminated photonic crystal structure is bright in color, has angle dependence and is suitable for large-scale preparation.
Drawings
FIG. 1 is a schematic structural diagram of a stacked photonic crystal with optical property control according to the present invention;
FIG. 2 is a scanning electron micrograph and UV-visible transmission spectra of a single-layer photonic crystal thin film prepared under different concentrations of 401nm colloidal microspheres prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image and an ultraviolet-visible transmission spectrum of a laminated (2-layer) photonic crystal thin film formed by stacking PMMA colloidal microspheres with particle sizes of 318 nm and 401nm prepared in example 2 of the present invention;
FIG. 4 is a scanning electron microscope image and UV-visible transmission spectrum of a laminated (2-layer) photonic crystal thin film formed by stacking PMMA colloidal microspheres with particle sizes of 454nm and 401nm prepared in example 3 of the present invention;
FIG. 5 is a scanning electron micrograph and UV-visible transmission spectra of stacked (3-layer) photonic crystals of PMMA colloidal microspheres with particle sizes of 318 nm, 401nm, and 454nm prepared in example 4 of the present invention;
FIG. 6 is a scanning electron micrograph and UV-visible transmission spectra of stacked (4-layer) photonic crystals of PMMA colloidal microspheres with particle sizes of 318 nm, 401nm, and 454nm prepared in example 5 of the present invention;
in the figure: 1 is a substrate, 2 is a pretreatment layer, and 3 is a laminated photonic crystal film.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments; all other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
[ example 1 ]
The method comprises the following steps: and (4) cleaning a crystallizing dish and a glass substrate used in the experiment, and drying for later use.
Step two: coating a layer of TiO 2-5nm thick on a glass substrate by spin coating2A film.
Step three: PMMA colloidal microspheres with the sphere diameter of 401nm are dispersed in water to prepare a solution with the concentration of 0.8 wt percent (1.0 wt percent), and the solution is placed in a crystallization dish to be fully stirred for 60 min for later use.
Step four: inserting the pretreated glass substrate into the crystallization dish containing the 401nm PMMA colloidal microsphere solution, and placing the crystallization dish at the temperature of 40 DEG CoAnd C, forming a single-layer photonic crystal film with a single spherical diameter (401 nm) on the substrate by adopting a flow control deposition method in a constant temperature and humidity box with the humidity of 65% RH.
Scanning Electron Microscope (SEM) characterization and ultraviolet-visible transmission spectrum analysis are carried out on the single-layer photonic crystal film, and the result is shown in FIG. 2. In fig. 2, a corresponds to a scanning electron microscope image of a single-layer photonic crystal film prepared from a colloidal microsphere solution with a concentration of 0.8 wt%, b corresponds to a scanning electron microscope image of a single-layer photonic crystal film prepared from a colloidal microsphere solution with a concentration of 1.0 wt%, and c corresponds to ultraviolet-visible transmission spectrums of two single-layer photonic crystal films. From the cross-section SEM photograph, it can be seen that the obvious unit photonic crystal thin film layer composed of 401nm PMMA colloidal microspheres, the arrangement of the microspheres is regular and ordered, the thickness of the thin film increases with the increase of the concentration of the colloidal microspheres, and in addition, the corresponding ultraviolet-visible transmission spectrogram shows that the photonic band gap intensity is enhanced with the increase of the thickness of the photonic crystal thin film, as shown in c in FIG. 2.
Specifically, the present embodimentIn the examples, the TiO2The film may also be applied by spraying or dip coating, in addition to TiO2The film can also be replaced by one of silicon dioxide, titanium dioxide, tungsten trioxide, vanadium pentoxide, zinc oxide, tin dioxide, cadmium sulfide, zinc sulfide, copper sulfide, bismuth vanadate, bismuth tungstate, strontium titanate, sodium tantalate, BiOBr, g-C3N4, polystyrene, polymethyl acrylate and polyacrylamide. The metal oxide film has good hydrophilicity and high flatness, and can be polymerized into multiple layers.
Specifically, in this embodiment, the monodisperse colloidal microsphere may be not only polymethyl methacrylate (PMMA), but also one of Polystyrene (PS), styrene-butyl acrylate-acrylic acid (PS-BA-AA) copolymer, Polyacrylamide (PAM), and silica.
Specifically, in the fourth step of this embodiment, the range of the parameters corresponding to the constant temperature and humidity environment of the constant temperature and humidity chamber may be 20-85 ℃ and 30-90% RH.
Specifically, in the fourth step of this embodiment, a single-layer photonic crystal thin film with a single microsphere size may be formed on the substrate by a vertical deposition or a dip coating method.
Specifically, in this embodiment, the glass substrate may be a flat glass or a curved glass, or may be one of quartz, a silicon wafer, a metal, a ceramic, a polymer, a fabric, and a flexible material.
[ example 2 ]
The method comprises the following steps: and (4) cleaning a crystallizing dish and a glass substrate used in the experiment, and drying for later use.
Step two: coating a layer of TiO 2-5nm thick on a glass substrate by spin coating2A film.
Step three: and (3) dispersing the PMMA colloidal microspheres with the sphere diameter of 318 nm in water to prepare a solution with the concentration of 0.45 wt%, and placing the solution in a crystallization dish to be fully stirred for 60 min for later use.
Step four: inserting the pretreated glass substrate into the crystallization dish containing 318 nm PMMA colloidal microsphere solution, and placing at the temperature of 40 DEG CoC, in a constant temperature and humidity box with the humidity of 65 percent RH, the sedimentation is controlled by adopting the flowAnd forming a first layer of unit photonic crystal thin film layer with a single spherical diameter size (318 nm) on the substrate by an integration method.
Step five: and (3) dispersing the PMMA colloidal microspheres with the sphere diameter of 401nm in water to prepare a solution with the concentration of 0.45 wt%, and placing the solution in a crystallization dish to be fully stirred for 60 min for later use.
Step six: coating a layer of TiO with the thickness of 1-3 nm on the 318 nm PMMA unit photonic crystal film obtained in the fourth step by adopting a spraying method2A film.
Step seven: and then inserting 318 nm PMMA colloidal microsphere solution prepared in the step IV, and repeating the step IV to obtain a laminated (2-layer) photonic crystal film with small spheres at the lower layer and large spheres at the upper layer on the glass substrate.
Scanning Electron Microscope (SEM) characterization and uv-vis transmission spectroscopy analysis were performed on the laminated (2-layer) photonic crystal thin film, and the results are shown in fig. 3. From the SEM photograph of the section a in FIG. 3, it can be seen that the boundary of the laminated unit photonic crystal thin film layer composed of 318 nm PMMA microspheres and the unit photonic crystal thin film layer composed of 401nm PMMA microspheres is obvious, and the microspheres are regularly and orderly arranged. The ultraviolet-visible transmission spectrogram shows that the photon forbidden band peak of the laminated (2-layer) photonic crystal film is formed by overlapping the photon forbidden bands of the unit photonic crystal film layers assembled by the colloidal microspheres with single size, as shown in b in figure 3.
Specifically, in this example, TiO in step two and step six2The film may also be coated by a dip coating, and in addition, TiO2The film can also be replaced by one of silicon dioxide, titanium dioxide, tungsten trioxide, vanadium pentoxide, zinc oxide, tin dioxide, cadmium sulfide, zinc sulfide, copper sulfide, bismuth vanadate, bismuth tungstate, strontium titanate, sodium tantalate, BiOBr, g-C3N4, polystyrene, polymethyl acrylate and polyacrylamide.
Specifically, in this embodiment, the monodisperse colloidal microspheres in step three and step five may be not only polymethyl methacrylate (PMMA), but also one of Polystyrene (PS), styrene-butyl acrylate-acrylic acid (PS-BA-AA) copolymer, Polyacrylamide (PAM), and silica.
Specifically, in the fourth step and the seventh step of this embodiment, the range of the parameters corresponding to the constant temperature and humidity environment of the constant temperature and humidity chamber may be 20-85 ℃ and 30-90% RH.
Specifically, in the fourth step and the seventh step of this embodiment, a single-layer photonic crystal film with a single microsphere size may be formed on the substrate by a vertical deposition or a dip coating method.
Specifically, in this embodiment, the glass substrate may be a flat glass or a curved glass, or may be one of quartz, a silicon wafer, a metal, a ceramic, a polymer, a fabric, and a flexible material.
[ example 3 ]
The method comprises the following steps: and (4) cleaning a crystallizing dish and a glass substrate used in the experiment, and drying for later use.
Step two: coating a layer of TiO 2-5nm thick on a glass substrate by spin coating2A film.
Step three: and (3) dispersing the PMMA colloidal microspheres with the sphere diameter of 454nm in water to prepare a solution with the concentration of 0.45 wt%, and placing the solution in a crystallization dish to be fully stirred for 60 min for later use.
Step four: inserting the pretreated glass substrate into the crystallization dish containing 454nm PMMA colloidal microsphere solution, and placing at the temperature of 40 DEG CoAnd C, forming a first layer of unit photonic crystal film layer with a single spherical diameter size (454 nm) on the substrate by adopting a flow control deposition method in a constant temperature and humidity box with the humidity of 65% RH.
Step five: and (3) dispersing the PMMA colloidal microspheres with the sphere diameter of 401nm in water to prepare a solution with the concentration of 0.45 wt%, and placing the solution in a crystallization dish to be fully stirred for 60 min for later use.
Step six: coating a layer of TiO with the thickness of 1-3 nm on the 454nm PMMA unit photonic crystal film obtained in the fourth step by adopting a spraying method2A film.
Step seven: and (4) inserting the 401nm PMMA colloidal microsphere solution prepared in the fifth step, repeating the fourth step, and obtaining a laminated (2-layer) photonic crystal film with big spheres on the lower layer and small spheres on the upper layer on the glass substrate.
Scanning Electron Microscope (SEM) characterization and uv-vis transmission spectroscopy analysis were performed on the laminated (2-layer) photonic crystal thin film, and the results are shown in fig. 4. From the SEM photograph of the section a in FIG. 4, it can be seen that the boundary of the laminated unit photonic crystal thin film layer composed of 454nm PMMA microspheres and the unit photonic crystal thin film layer composed of 401nm PMMA microspheres is obvious, and the microspheres are regularly and orderly arranged. The ultraviolet-visible transmission spectrogram shows that the photon forbidden band peak of the laminated (2-layer) photonic crystal film is formed by overlapping the photon forbidden bands of the unit photonic crystal film layers assembled by the colloidal microspheres with single size, as shown in b in fig. 4.
Specifically, in this example, TiO in step two and step six2The film may also be coated by a dip coating, and in addition, TiO2The film can also be replaced by one of silicon dioxide, titanium dioxide, tungsten trioxide, vanadium pentoxide, zinc oxide, tin dioxide, cadmium sulfide, zinc sulfide, copper sulfide, bismuth vanadate, bismuth tungstate, strontium titanate, sodium tantalate, BiOBr, g-C3N4, polystyrene, polymethyl acrylate and polyacrylamide.
Specifically, in this embodiment, the monodisperse colloidal microspheres in step three and step five may be not only polymethyl methacrylate (PMMA), but also one of Polystyrene (PS), styrene-butyl acrylate-acrylic acid (PS-BA-AA) copolymer, Polyacrylamide (PAM), and silica.
Specifically, in the second step and the sixth step of this embodiment, the range of the parameters corresponding to the constant temperature and humidity environment of the constant temperature and humidity chamber may be 20-85 ℃ and 30-90% RH.
Specifically, in the fourth step and the seventh step of this embodiment, a single-layer photonic crystal film with a single microsphere size may be formed on the substrate by a vertical deposition or a dip coating method.
Specifically, in this embodiment, the glass substrate may be a flat glass or a curved glass, or may be one of quartz, a silicon wafer, a metal, a ceramic, a polymer, a fabric, and a flexible material.
[ example 4 ]
The method comprises the following steps: and (4) cleaning a crystallizing dish and a glass substrate used in the experiment, and drying for later use.
Step two: coating a layer of TiO 2-5nm thick on a glass substrate by spin coating2A film.
Step three: and (3) dispersing the PMMA colloidal microspheres with the sphere diameter of 318 nm in water to prepare a solution with the concentration of 0.45 wt%, and placing the solution in a crystallization dish to be fully stirred for 60 min for later use.
Step four: inserting the pretreated glass substrate into the crystallization dish containing 318 nm PMMA colloidal microsphere solution, and placing at the temperature of 40 DEG CoAnd C, forming a first layer of unit photonic crystal thin film layer with a single sphere diameter size (318 nm) on the substrate by adopting a flow control deposition method in a constant temperature and humidity box with the humidity of 65% RH.
Step five: and (3) dispersing the PMMA colloidal microspheres with the sphere diameter of 401nm in water to prepare a solution with the concentration of 0.45 wt%, and placing the solution in a crystallization dish to be fully stirred for 60 min for later use.
Step six: coating a layer of TiO with the thickness of 1-3 nm on the 318 nm PMMA unit photonic crystal film obtained in the fourth step by adopting a spraying method2A film.
Step seven: and (3) inserting the 401nm PMMA colloidal microsphere solution prepared in the fifth step, repeating the fourth step, and obtaining a laminated (2-layer) photonic crystal film with small spheres at the lower layer and large spheres at the upper layer on the glass substrate.
Step eight: and (3) dispersing the PMMA colloidal microspheres with the sphere diameter of 454nm in water to prepare a solution with the concentration of 0.45 wt%, and placing the solution in a crystallization dish to be fully stirred for 60 min for later use.
Step nine: coating a layer of TiO with the thickness of 1-3 nm on the 318/401 nm PMMA double-layer superposed photonic crystal film obtained in the sixth step by adopting a spraying method2A film.
Step ten: and (3) inserting the 454nm PMMA colloidal microsphere solution prepared in the step eight, repeating the step four, and obtaining a laminated (3-layer) photonic crystal film with the size of the microspheres overlapped from small to large on the glass substrate.
Scanning Electron Microscope (SEM) characterization was performed on the laminated (3-layer) photonic crystal thin film, and the results are shown in fig. 5. From the SEM photograph of the section a in FIG. 5, it can be seen that the boundary lines of the unit photonic crystal thin film layer stacks respectively composed of 318 nm PMMA microspheres, 401nm PMMA microspheres and 454 nmPMMMA microspheres are obvious, and the microspheres are regularly and orderly arranged. The ultraviolet-visible transmission spectrogram shows that the photon forbidden band peak of the laminated (3-layer) photonic crystal film is formed by overlapping the photon forbidden bands of the unit photonic crystal film layers assembled by the colloidal microspheres with single size, as shown in b in fig. 5.
Specifically, in this example, TiO in step two, step six, and step nine2The film may also be coated by a dip coating, and in addition, TiO2The film can also be replaced by one of silicon dioxide, titanium dioxide, tungsten trioxide, vanadium pentoxide, zinc oxide, tin dioxide, cadmium sulfide, zinc sulfide, copper sulfide, bismuth vanadate, bismuth tungstate, strontium titanate, sodium tantalate, BiOBr, g-C3N4, polystyrene, polymethyl acrylate and polyacrylamide.
Specifically, in this embodiment, the monodisperse colloidal microspheres in the third step, the fifth step and the eighth step may be not only polymethyl methacrylate (PMMA), but also one of Polystyrene (PS), styrene-butyl acrylate-acrylic acid (PS-BA-AA) copolymer, Polyacrylamide (PAM) and silica.
Specifically, in the second step, the sixth step and the tenth step of this embodiment, the parameter range corresponding to the constant temperature and humidity environment of the constant temperature and humidity chamber may be 20 to 85 ℃ and 30 to 90% RH.
Specifically, in the second step, the sixth step and the tenth step of this embodiment, a single-layer photonic crystal film with a single microsphere size may be formed by self-assembly on the substrate through a vertical deposition or a dip coating method.
Specifically, in this embodiment, the glass substrate may be a flat glass or a curved glass, or may be one of quartz, a silicon wafer, a metal, a ceramic, a polymer, a fabric, and a flexible material.
[ example 5 ]
The method comprises the following steps: and (4) cleaning a crystallizing dish and a glass substrate used in the experiment, and drying for later use.
Step two: coating a layer of TiO 2-5nm thick on a glass substrate by spin coating2A film.
Step three: and (3) dispersing the PMMA colloidal microspheres with the sphere diameter of 318 nm in water to prepare a solution with the concentration of 0.45 wt%, and placing the solution in a crystallization dish to be fully stirred for 60 min for later use.
Step four: inserting the pretreated glass substrate into the crystallization dish containing 318 nm PMMA colloidal microsphere solution, and placing at the temperature of 40 DEG CoAnd C, forming a first layer of unit photonic crystal film layer with a single sphere diameter size (401 nm) on the substrate by adopting a flow control deposition method in a constant temperature and humidity box with the humidity of 65% RH.
Step five: soaking the photonic crystal film in the fourth step into TiO2Drying and calcining the solution to obtain TiO with the aperture of 248 nm2An inverse opal unit photonic crystal thin film layer.
Step six: and (3) dispersing the PMMA colloidal microspheres with the sphere diameter of 318 nm in water to prepare a solution with the concentration of 0.45 wt%, and placing the solution in a crystallization dish to be fully stirred for 60 min for later use.
Step seven: the TiO obtained in the fifth step2And (3) inserting the unit inverse proteolith photonic crystal film into the 318 nm PMMA colloidal microsphere solution prepared in the sixth step, repeating the fourth step, and obtaining the laminated (2-layer) photonic crystal film on the glass substrate.
Step eight: 248 nmTiO obtained in step seven by spraying2Coating a layer of TiO with the thickness of 1-3 nm on the inverse opal/318 nm PMMA double-layer superposed photonic crystal film2A film.
Step nine: and (3) dispersing the PMMA colloidal microspheres with the sphere diameter of 401nm in water to prepare a solution with the concentration of 0.45 wt%, and placing the solution in a crystallization dish to be fully stirred for 60 min for later use. Then the photonic crystal film obtained in the step eight is inserted into the solution, the step four is repeated, and 248 nm TiO is obtained on the glass substrate2Inverse opal/318/401 nm PMMA (3 layer) photonic crystal film.
Step ten: 248 nm TiO obtained in the ninth step by adopting a spraying method2Inverse opal/318/401 nm PMMA (3 layers) photonic crystal is coated with a 1-3 nm thick layer of TiO2A film.
Step eleven: particle size reductionThe 454nm PMMA colloidal microspheres are dispersed in water to prepare a solution with the concentration of 0.45 wt%, and the solution is placed in a crystallization dish to be fully stirred for 60 min for later use. Then the photonic crystal film obtained in the step ten is inserted into the solution, the step four is repeated, and 248 nm TiO is obtained on the glass substrate2Inverse opal/318/401/454 nm PMMA (four layer) photonic crystal film.
Specifically, other process parameters in the present embodiment are the same as those in the other embodiments.
In addition, in this embodiment, according to design requirements, a nano-planarization pretreatment method and colloidal microsphere self-assembly may be further performed on the four layers of photonic crystal films obtained in step eleven to obtain five or more layers of stacked photonic crystals.
Scanning Electron Microscope (SEM) characterization was performed on the above laminated (4-layer) photonic crystal film, and the result is shown as a in fig. 6. The section SEM photograph shows that the boundary of the four-layer unit photonic crystal film layer is obvious, and the microsphere/cavity arrangement is regular and ordered. The ultraviolet-visible transmission spectrum is shown as b in fig. 6.
Therefore, the laminated photonic crystal with optical performance regulation and control prepared by the method has the structure shown in fig. 1, and comprises a substrate 1, wherein a nano thin film layer 2 is arranged on the substrate, a plurality of unit photonic crystal thin film layers 3 are arranged on the nano thin film layer 2, the nano thin film layer 2 is also arranged between each unit photonic crystal thin film layer 3, and the plurality of unit photonic crystal thin film layers 3 are formed by self-assembling colloidal microspheres with single microsphere size. That is to say, the laminated photonic crystal of the application is formed by stacking a plurality of layers of unit photonic crystal films on a substrate layer by layer, the photonic band gap peak in the ultraviolet-visible transmission spectrum is formed by overlapping the photonic band gaps of the unit photonic crystal film layers assembled by colloidal microspheres with single size, each layer of single-component photonic crystal film is formed by self-assembling the colloidal microspheres with single microsphere size, and the sizes of the corresponding colloidal microspheres of different layers can be the same or different.
In summary, the stable laminated photonic crystal structure is obtained by multilayer assembly of colloidal particles with different sizes, so that any order stacking of unit photonic crystal films with different sizes can be realized, and the number of stacked layers has no upper limit theoretically. The optical performance of the material can realize optical regulation and control in an ultraviolet-visible-infrared full spectrum range, realizes absorption and reflection of different wavelengths of light, can regulate and control the absorption of different wavelengths of light, and has wide application potential in the aspects of photoelectrocatalysis, solar water decomposition, bionic materials, anti-counterfeiting marks, solar cells and the like. The method is simple to operate, short in time consumption, capable of controlling the number of layers, bright in color of the prepared structure, angle-dependent and suitable for large-scale preparation.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. The laminated photonic crystal with the optical performance regulation function is characterized by comprising a substrate (1), wherein a nano thin film layer (2) is arranged on the substrate (1), a plurality of layers of unit photonic crystal thin film layers (3) are arranged on the nano thin film layer (2), the nano thin film layer (2) is also arranged between every two layers of unit photonic crystal thin film layers (3), and the plurality of layers of unit photonic crystal thin film layers (3) are formed by self-assembly of colloidal microspheres with single microsphere sizes.
2. The laminated photonic crystal with optical performance regulation and control function as claimed in claim 1, wherein the number of the unit photonic crystal thin film layers (3) is 2-4; the material of the nano film layer (2) is one of silicon dioxide, titanium dioxide, tungsten trioxide, vanadium pentoxide, zinc oxide, tin dioxide, cadmium sulfide, zinc sulfide, copper sulfide, bismuth vanadate, bismuth tungstate, strontium titanate, sodium tantalate, BiOBr, g-C3N4, polystyrene, polymethyl acrylate and polyacrylamide, the thickness of the nano film layer (2) arranged on the substrate (1) is 2-5nm, and the thickness of the nano film layer (2) between the unit photonic crystal film layers (3) is 1-3 nm.
3. A preparation method of laminated photonic crystals with optical performance regulation and control is characterized in that a monodisperse colloidal microsphere is used for self-assembly on a substrate subjected to nano-level pretreatment to prepare a unit photonic crystal thin film layer; and then carrying out nano leveling pretreatment on the unit photonic crystal thin film layer, then carrying out self-assembly by using the monodisperse colloidal microspheres again, and carrying out the nano leveling pretreatment and the self-assembly of the monodisperse colloidal microspheres for multiple times in a circulating manner to form a laminated photonic crystal film formed by stacking multiple layers of unit photonic crystal thin films layer by layer, wherein each layer of unit photonic crystal thin film is formed by self-assembly of colloidal microspheres with single size.
4. The method for preparing the laminated photonic crystal with optical property regulation and control as claimed in claim 3, characterized by comprising the following steps:
s1, soaking and cleaning the container and the substrate containing the colloidal microsphere solution, and then washing the container and the substrate clean by distilled water for later use;
s2, dissolving monodisperse colloidal microspheres with single microsphere size in a solvent, fully stirring and dispersing to prepare 0.02-3wt% colloidal microsphere solution for later use;
s3, performing nano-grade pretreatment on the cleaned substrate;
s4, inserting the pretreated substrate into the colloidal microsphere solution, placing the solution in a constant temperature and humidity environment, and self-assembling the solution on the substrate to form a unit photonic crystal thin film layer with a single microsphere size;
s5, replacing monodisperse colloid microsphere solutions with different sizes and concentrations, and repeating the steps S2-S4 for multiple times to obtain the laminated photonic crystal film.
5. The method according to claim 4, wherein in step S3, the nano-planarization pre-treatment method is spin coating, spray coating or lift coating, and the nano-film material comprises a metal compound and a polymer, and the metal compound is one of silicon dioxide, titanium dioxide, tungsten trioxide, vanadium pentoxide, zinc oxide, tin dioxide, cadmium sulfide, zinc sulfide, copper sulfide, bismuth vanadate, bismuth tungstate, strontium titanate, sodium tantalate, BiOBr, g-C3N4, polystyrene, polymethyl acrylate, and polyacrylamide.
6. The method for preparing a laminated photonic crystal with optical property control according to claim 4, wherein in step S2, the monodisperse colloidal microsphere is one of polymethyl methacrylate (PMMA), Polystyrene (PS), styrene-butyl acrylate-acrylic acid (PS-BA-AA) copolymer, Polyacrylamide (PAM), and silica; the solvent is water.
7. The method for preparing a laminated photonic crystal with adjustable optical properties as claimed in claim 4, wherein in step S4, the constant temperature and humidity environment has parameters of 20-85 ℃ and 30-90% RH.
8. The method of claim 4, wherein in step S4, the single microsphere-sized photonic crystal unit film is formed by self-assembly on a substrate through vertical deposition, flow control deposition or Czochralski coating.
9. The method for preparing a laminated photonic crystal with optical property regulation and control as claimed in claim 3, wherein the substrate is one of planar glass, curved glass, quartz, silicon wafer, metal, ceramic, polymer, fabric, and flexible material.
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