CN115785496A - Double-layer thermal response photonic crystal thin film device and preparation method thereof - Google Patents
Double-layer thermal response photonic crystal thin film device and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a double-layer thermal response photonic crystal thin film device and a preparation method thereof. The preparation method comprises the following steps: firstly assembling a photonic crystal template, mixing a color developing agent, a leuco agent, a solvent, polydimethylsiloxane, a curing agent and a diluent, dripping the mixture on the surface of a glass substrate, carrying out high-temperature thermosetting to obtain a thermochromic polymer film, transferring the photonic crystal template into the thermochromic polymer film, combining the thermochromic polymer film with a blank glass substrate, penetrating a polymer precursor solution into a gap between the two glass substrates, standing, and stripping the glass substrate after high-temperature thermosetting to obtain the photochromic polymer film. The invention uses the thermochromic polymer film with melting darkening or melting brightening as the switch of the photonic crystal film optical path, and the obtained photonic crystal film has hydrophobicity, corrosion resistance and high stability.
Description
Technical Field
The invention relates to a crystal film and a preparation method thereof, in particular to a double-layer thermal response photonic crystal film device and a preparation method thereof.
Background
The response type photonic crystal is an intelligent response material for dynamically tuning electromagnetic wave propagation, can convert external stimuli such as heat, light, humidity, ion concentration, magnetic field and the like into optical signals and structural color changes, and has wide application prospects in the aspects of anti-counterfeiting, sensing, displays, green printing, photocatalysis and the like. One of the methods for constructing a responsive composite material is to prepare a responsive photonic crystal based on responsive assembly units. The thermal response photonic crystal has a huge application prospect due to the fact that the thermal response photonic crystal is easy to construct. Generally, the response type photonic crystal realizes the tunable response of the structure by adjusting the periodic lattice constant of the photonic crystal, such as the refractive index of the material, the incident light angle, the lattice spacing and the like to cause the red shift or the blue shift of the reflection peak. Achieving a photonic crystal's stimulus response by adjusting non-array parameters is therefore a significant challenge.
The organic thermochromic phase change system has better performance and is a three-component organic thermochromic phase change system with better prospect. The system is mainly composed of a color developing agent for initiating thermochromism, a leuco agent for providing thermochromism groups and a solvent for determining the color-changing temperature. The color-developing agents are mainly classified into fluorans, triarylmethanes, spiropyrans and the like, such as crystal violet lactone CVL, and the leuco agents mainly comprise phenols, ethers, ketones, esters and the like, and are commonly bisphenol A, bisphenol S, alkyl gallate and the like. Researches show that the shade of the color after color change is related to both a color developing agent and a solvent: song et al studied the thermochromic behavior of a thermo-sensitive green/bisphenol AF/dodecanol solvent system, and found that the system has reversible thermochromic behavior, is green in the crystalline state and decolors in the molten state; tang et al have studied the crystal violet lactone/lauryl gallate/dodecanol solvent system to find that there is no discoloration, while crystal violet lactone/lauryl gallate/tetradecanol have reversible thermochromic properties, and appear blue in the molten state and colorless in the crystalline state.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a double-layer thermal response photonic crystal thin film device with hydrophobicity, corrosion resistance and high stability;
the second purpose of the invention is to provide a preparation method of the double-layer thermal response photonic crystal thin film device.
The technical scheme is as follows: the double-layer thermal response photonic crystal thin film device comprises a thermochromic polymer film, an opal photonic crystal thin film assembled by nano microspheres and a polymer thin film material filled in the opal photonic crystal thin film, wherein the thermochromic polymer film, the opal photonic crystal thin film and the polymer thin film material form a sandwich structure; the thermochromic polymer film is formed by curing a thermochromic phase change system and a polymer precursor solution at high temperature; the polymer film material is formed by high-temperature curing of a precursor solution consisting of polydimethylsiloxane, a curing agent and a diluent.
Wherein the thickness of the thermochromic polymer film is 50-100 μm, and the thickness of the opal photonic crystal film is 10-50 μm.
Wherein the particle size of the nano-microsphere is 150nm-550nm.
The nano-microsphere is one of silicon dioxide, titanium dioxide, tin dioxide, polystyrene, polymethyl methacrylate, cadmium sulfide, zinc oxide or silicon dioxide coated polystyrene, polymethyl methacrylate or titanium dioxide coated poly (styrene-methyl methacrylate-acrylic acid) polymer colloidal microsphere or silicon dioxide coated zinc oxide, cadmium sulfide and titanium dioxide.
The preparation method of the double-layer thermal response photonic crystal thin film device comprises the following steps:
(1) Assembling a photonic crystal template from the nano microspheres by a vertical deposition method;
(2) Mixing a color developing agent, a leuco agent, a solvent, polydimethylsiloxane, a curing agent and a diluent, then dripping the mixture on the surface of a glass substrate, and carrying out high-temperature thermal curing to obtain a thermochromic polymer film;
(3) Transferring the photonic crystal template in the step (1) into a thermochromic polymer film to obtain a glass substrate;
(4) Combining the glass substrate and the blank glass substrate in the step (3), permeating a polymer precursor solution from the gap between the two glass substrates under the capillary action, standing to enable the polymer precursor solution to permeate into opal pores, and performing high-temperature thermal curing; the polymer precursor solution comprises polydimethylsiloxane, a curing agent and a diluent;
(5) And stripping the glass substrate to obtain the double-layer thermal response photonic crystal film.
Wherein in the step (4), the volume ratio of the polydimethylsiloxane, the curing agent and the diluent is 0.1-0.3.
Wherein, in the step (1), the concentration of the vertical deposition solution is 0.5-2wt%
Wherein, in the step (2), the molar ratio of the color developing agent, the leuco agent and the solvent is 1-3:1-3;
wherein in the step (2), the mass ratio of the thermochromic phase change system, the diluent polymer, the polydimethylsiloxane and the curing agent is 0.05-0.1.
Wherein, the color developing agent is phenols, sulfonic acids, carboxylic acids, halohydrins and derivatives thereof;
wherein the leuco agent is one of triarylmethanes, phenothiazines, fluorans, spiropyran or rhodamine B lactams; the solvent is alcohol, ether, ketone, phosphate, carboxylate, sulfonate, sulfite and the like, and the diluent is one of alcohol, hydrocarbon, ether or ketone.
The invention principle is as follows: the temperature is used for regulating and controlling the thermochromic polymer film to cause the photonic crystal optical path to be displayed or hidden, so that the double-layer thermal response photonic crystal film can be applied to the fields of anti-counterfeiting and intelligent windows. Compared with the traditional response type photonic crystal, the double-layer photonic crystal realizes stimulation response through non-array parameter regulation and control, has no volume change in the response process, uses the polymer closed nano microsphere photonic crystal, can improve the friction resistance and solvent resistance of the photonic crystal device, and is beneficial to widening the application field of the photonic crystal device.
Has the advantages that: compared with the prior art, the invention has the following remarkable effects: 1. the thermochromic polymer film with melting darkening or melting brightening is used as a switch of an optical path of the photonic crystal film, and the obtained photonic crystal film has hydrophobicity, corrosion resistance and high stability. 2. Self-cleaning can be achieved, and color effects of permanent fade and angle dependence are achieved. 3. Simple process and low cost. 4. The color change of the color fading of the thermochromic film can be realized by heating, and the optical path of the photonic crystal is opened, so that the information display is realized. 5. Accessible illumination makes the device temperature rise, obtains the effect that the colour deepens to realize thermal-insulated, energy saving's effect, the existence of photonic crystal can absorb most ultraviolet light, plays the effect of ultraviolet protection, can be applied to smart window.
Drawings
FIG. 1 is a flow chart of the fabrication of a thermally responsive double-layer photonic crystal thin film device in accordance with the present invention;
FIG. 2 is a SEM image of a polystyrene microsphere template of example 1, a reflectance spectrum of a diffuse reflectance spectrum detected by an integrating sphere mode, and a corresponding optical microscope photograph;
FIG. 3 is a SEM image of a polystyrene microsphere template of example 2, a reflectance spectrum of diffuse reflectance spectrum detected by an integrating sphere mode, and a corresponding optical micrograph;
FIG. 4 is a SEM image of a polystyrene microsphere template of example 3, a reflectance spectrum of diffuse reflectance spectrum detected by an integrating sphere mode, and a corresponding optical micrograph;
FIG. 5 is a SEM image of a polystyrene microsphere template of example 4, a reflectance spectrum of a diffuse reflectance spectrum detected using an integrating sphere mode, and a corresponding optical micrograph;
FIG. 6 is an optical photograph of the melt-brightened two-layer thermally responsive photonic crystal film in the molten state and an optical photograph of the photonic crystal film in the crystalline state in example 2;
FIG. 7 is a digital photograph of a polystyrene template as a function of angle of incidence in example 3;
FIG. 8 is an angle-dependent reflectance spectrum of the photonic crystal thin film prepared in example 3;
FIG. 9 is an optical photograph of the melt-darkening thermochromic phase-change system of example 4;
FIG. 10 is a reflection spectrum of a thermally responsive photonic crystal film in example 3;
FIG. 11 is an optical photograph of the photonic crystal prepared in comparative example 1;
FIG. 12 is an optical photograph of the photonic crystal prepared in comparative example 2;
FIG. 13 is an optical photograph of the thermochromic system of comparative example 3.
Detailed Description
The present invention is described in further detail below.
Example 1
A double-layer thermal response photonic crystal thin film device is prepared by the following steps:
(1) Mixing crystal violet lactone, bisphenol A and hexadecanol according to a molar ratio of 1.
(2) And assembling the polystyrene opal photonic crystal template with the grain size of 183nm by a vertical deposition method in a constant-temperature drying oven with the temperature of 60 ℃ and the humidity of 50 percent, wherein the solid content of the deposition liquid is 0.5 percent by weight. The preassembled photonic crystal template is carefully transferred into the thermochromic polymer film described above.
(3) Combining the glass substrate and the blank glass substrate in the last step, pouring a polymer precursor solution mixed according to the volume ratio of Sylgard184 polydimethylsiloxane, sylgard184 curing agent and diluent of 0.2.
FIG. 1 is a flow chart of the fabrication of a thermally responsive bilayer photonic crystal thin film device according to this embodiment, and is applicable to all embodiments. The double-layer photonic crystal thin film device is prepared by a three-step method, namely, a thermochromic polymer film is firstly prepared, a polystyrene opal photonic crystal is preassembled, a photonic crystal template is transferred to the thermochromic polymer film and then is combined with another glass substrate, a polymer precursor is filled in a gap between two glass plates, and the photonic crystal thin film is obtained by high-temperature thermocuring.
FIG. 2 is a SEM image of the-183 nm polystyrene microsphere template used in this example, and the top right corner of a in FIG. 2 is the corresponding fast Fourier transform spectrum; b in FIG. 2 is a reflection spectrum of diffuse reflection spectrum detected by integrating sphere mode; in FIG. 2, c is the corresponding optical micrograph, and in the digital photograph, the film is purple.
Example 2
A double-layer thermal response photonic crystal thin film device is prepared by the following steps:
(1) Mixing crystal violet lactone, bisphenol S and hexadecanol according to a molar ratio of 1.
(2) Assembling the polystyrene opal photonic crystal template with the grain size of 210nm by a vertical deposition method in a constant-temperature drying oven with the temperature of 60 ℃ and the humidity of 50 percent, wherein the solid content of the deposition solution is 1wt percent. The preassembled photonic crystal template is carefully transferred into the thermochromic polymer film described above.
(3) Combining the glass substrate and the blank glass substrate in the previous step, pouring a polymer precursor solution mixed according to the volume ratio of Sylgard184 polydimethylsiloxane, sylgard184 curing agent and diluent of 0.2.
FIG. 3 is a SEM image of the polystyrene microsphere template of-210 nm used in this example, and the top right corner of a in FIG. 3 is the corresponding fast Fourier transform spectrum; b in FIG. 3 is a reflection spectrum of diffuse reflection spectrum detected by integrating sphere mode; in fig. 3 c is the corresponding optical micrograph, and in the digital photograph the film is green.
Fig. 6 a is an optical photograph of the double-layer thermally responsive photonic crystal film in a molten state in the present embodiment, and fig. 6 b is an optical photograph of the double-layer thermally responsive photonic crystal film in a crystalline state.
Example 3
A double-layer thermal response photonic crystal thin film device is prepared by the following steps:
(1) Mixing crystal violet lactone, bisphenol A and hexadecanol according to a molar ratio of 1.
(2) Assembling the polystyrene opal photonic crystal template with the grain size of 249nm by a vertical deposition method in a constant-temperature drying oven with the temperature of 60 ℃ and the humidity of 50 percent, wherein the solid content of the deposition solution is 2 weight percent. The preassembled photonic crystal template is carefully transferred into the thermochromic polymer film described above.
(3) Combining the glass substrate and the blank glass substrate in the previous step, pouring a polymer precursor solution mixed according to the volume ratio of Sylgard184 polydimethylsiloxane, sylgard184 curing agent and diluent of 0.2.
In FIG. 4, a is an SEM image of a 249nm polystyrene microsphere template used in the example, and the upper right corner of a in FIG. 4 is a corresponding fast Fourier transform spectrum; b in FIG. 4 is a reflection spectrum of diffuse reflection spectrum detected by integrating sphere mode; in fig. 4 c is the corresponding microscope photo, in which the film is orange.
Fig. 7 is a digital photograph of the polystyrene opal photonic crystal template in this embodiment, taken with the change of the incident angle, where the positions of the light source and the camera are fixed, and the incident angles are 0 °, 10 °, 30 °, 45 °, 60 °, and 90 °, respectively. The photograph shows the structural color changing from orange to blue.
Fig. 8 shows a reflection spectrum of the photonic crystal film of the present example after filling the polystyrene opal photonic crystal with PDMS, the reflection peak is 649nm when the observation angle is 0 °, the reflection peak is blue shifted with the increase of the observation angle, and the reflection peak wavelength is 495nm when the observation angle is 80 °.
Example 4
A double-layer thermal response photonic crystal thin film device is prepared by the following steps:
(1) Mixing crystal violet lactone, lauryl gallate and tetradecanol according to a molar ratio of 1.
(2) Assembling the polystyrene opal photonic crystal template with the grain size of 263nm by a vertical deposition method in a constant-temperature drying oven with the temperature of 60 ℃ and the humidity of 50 percent, wherein the solid content of the deposition liquid is 1wt percent. The preassembled photonic crystal template is carefully transferred into the thermochromic polymer film described above.
(3) Combining the glass substrate and the blank glass substrate in the previous step, pouring a polymer precursor solution mixed according to the volume ratio of Sylgard184 polydimethylsiloxane, sylgard184 curing agent and diluent of 0.1.
FIG. 5 is a SEM image of the-263 nm polystyrene microsphere template used in this example, and the top right corner of a in FIG. 5 is the corresponding fast Fourier transform spectrum; in fig. 5, b is a reflectance spectrum of diffuse reflectance spectrum detected by integrating sphere mode, c in fig. 5 is a corresponding optical photograph of microscope, and the film is red in digital photograph.
Fig. 9 shows the color change of the melting darkening type thermochromic phase change system in this example, which shows a significant phenomenon of color depth upon heating under the conditions of high developer concentration, low solvent concentration, and matching of developer and solvent alkyl chain length.
Example 5
A double-layer thermal response photonic crystal thin film device is prepared by the following steps:
(1) Mixing crystal violet lactone, bisphenol A and hexadecanol according to a molar ratio of 1.
(2) A patterned PDMS mask is pasted on a glass substrate cleaned by piranha solution, a patterned polystyrene opal photonic crystal template with the grain size of 210nm is assembled by a vertical deposition method in a constant-temperature drying box with the temperature of 60 ℃ and the humidity of 50%, and the solid content of a deposition solution is 1wt%. The pre-assembled patterned photonic crystal template was carefully transferred into the thermochromic polymer film described above.
(3) Combining the glass substrate and the blank glass substrate in the previous step, pouring a polymer precursor mixed according to the volume ratio of Sylgard184 polydimethylsiloxane, sylgard184 curing agent and diluent of 0.1.
Fig. 10 is a reflection spectrogram of the thermally responsive photonic crystal film in this example, which is sequentially a reflection spectrogram when observed from the side of the thermochromic polymer film in a crystalline state, and a reflection spectrogram when observed from the side of the photonic crystal film in a crystalline state. A reflection spectrum when observed from the side of the thermochromic polymer film in a molten state, and a reflection spectrum when observed from the side of the photonic crystal film in a molten state.
Comparative example 1
A double-layer thermal response photonic crystal thin film device is prepared by the following steps:
(1) Mixing crystal violet lactone, bisphenol A and tetradecanol according to a molar ratio of 1.
(2) Assembling the polystyrene opal photonic crystal template with the grain size of 210nm by a vertical deposition method in a constant-temperature drying oven with the temperature of 80 ℃ and the humidity of 50 percent, wherein the solid content of the deposition solution is 1 weight percent. The preassembled photonic crystal template is carefully transferred into the thermochromic polymer film described above.
(3) Combining the glass substrate and the blank glass substrate in the previous step, pouring a polymer precursor mixed according to the volume ratio of Sylgard184 polydimethylsiloxane, sylgard184 curing agent and diluent of 0.1.
FIG. 11 is an optical photograph of the photonic crystal prepared in comparative example 1, in which the deposition time was insufficient due to the excessively high assembly temperature, and the regularity of the obtained photonic crystal film was poor.
Comparative example 2
A double-layer thermal response photonic crystal thin film device is prepared by the following steps:
(1) Mixing crystal violet lactone, bisphenol A and hexadecanol according to a molar ratio of 1.
(2) And assembling the polystyrene opal photonic crystal template with the grain size of 210nm by a vertical deposition method in a constant-temperature drying oven with the temperature of 60 ℃ and the humidity of 50 percent, wherein the solid content of the deposition solution is 3wt percent. The preassembled photonic crystal template is carefully transferred into the thermochromic polymer film described above.
(3) Combining the glass substrate and the blank glass substrate in the previous step, pouring a polymer precursor solution mixed according to the volume ratio of Sylgard184 polydimethylsiloxane, sylgard184 curing agent and diluent of 0.1.
FIG. 12 is a photo of the photonic crystal prepared in comparative example 2, in which the thickness of the photonic crystal film is large due to the high concentration of the assembly liquid, and the photonic crystal is largely detached due to the weak bonding force with the glass substrate.
Comparative example 3
A double-layer thermal response photonic crystal thin film device is prepared by the following steps:
(1) Mixing crystal violet lactone, octadecyl gallate and tetradecanol according to a molar ratio of 1.
(2) Assembling the polystyrene opal photonic crystal template with the grain size of 263nm by a vertical deposition method in a constant-temperature drying oven with the temperature of 60 ℃ and the humidity of 50 percent, wherein the solid content of the deposition liquid is 0.5 percent by weight. The preassembled photonic crystal template is carefully transferred into the thermochromic polymer film described above.
(3) Combining the glass substrate and the blank glass substrate in the last step, pouring a polymer precursor solution mixed according to the volume ratio of Sylgard184 polydimethylsiloxane, sylgard184 curing agent and diluent of 0.1.
Fig. 13 shows the thermochromic performance of the thermochromic system in comparative example 3, and comparative example 3 fails to show a melt-darkening discoloration effect and the color change is not significant due to the high solvent concentration, mismatch of the solvent and the developer alkyl chain length.
The experiments show that the photonic crystal film with a regular structure and an obvious structural color can be obtained by controlling the deposition conditions of the photonic crystal, such as deposition temperature and concentration of deposition liquid, the thermochromic polymer film with obvious color change and good color change sensitivity is prepared by adjusting the volume ratio of the components of the thermochromic phase change system, the polymer film and the photonic crystal film are assembled by polydimethylsiloxane to prepare the double-layer thermally responsive photonic crystal film with good thermal responsiveness, the lower structural color is displayed and hidden by the color change of the upper thermochromic polymer film under the temperature stimulation, and the colorful high-quality intelligent product is prepared by the synergistic effect of the structural color and the color of the pigment color.
Claims (10)
1. A double-layer thermal response photonic crystal thin film device is characterized by comprising a thermochromic polymer film, an opal photonic crystal thin film assembled by nano microspheres and a polymer thin film material filled in the opal photonic crystal thin film, wherein the thermochromic polymer film, the opal photonic crystal thin film and the polymer thin film material form a sandwich structure; the thermochromic polymer film is formed by curing a thermochromic phase change system and a polymer precursor solution at high temperature; the polymer film material is formed by curing a precursor solution consisting of polydimethylsiloxane, a curing agent and a diluent at high temperature.
2. The bilayer thermally responsive photonic crystal thin film device of claim 1, wherein said thermochromic polymer film has a thickness of 50-100 μm and said opal photonic crystal thin film has a thickness of 10-50 μm.
3. The bilayer thermally responsive photonic crystal thin film device of claim 1, wherein said nanovesicles have a particle size of 150nm to 550nm.
4. The bilayer thermally responsive photonic crystal thin film device of claim 1, wherein the nanospheres are one of silica, titanium dioxide, tin dioxide, polystyrene, polymethyl methacrylate, cadmium sulfide, zinc oxide, or silica-coated polystyrene, polymethyl methacrylate, or titanium dioxide-coated poly (styrene-methyl methacrylate-acrylic acid) polymer colloidal microspheres, or silica-coated zinc oxide, cadmium sulfide, or titanium dioxide.
5. A method for preparing a bilayer thermal response photonic crystal thin film device of claim 1, comprising the steps of:
(1) Assembling a photonic crystal template from the nano-microspheres by a vertical deposition method;
(2) Mixing a color developing agent, a leuco agent, a solvent, polydimethylsiloxane, a curing agent and a diluent, then dripping the mixture on the surface of a glass substrate, and carrying out high-temperature thermal curing to obtain a thermochromic polymer film;
(3) Transferring the photonic crystal template in the step (1) into a thermochromic polymer film to obtain a glass substrate;
(4) Combining the glass substrate and the blank glass substrate in the step (3), permeating a polymer precursor solution from the gap between the two glass substrates under the capillary action, standing to enable the polymer precursor solution to permeate into opal pores, and performing high-temperature thermal curing; the polymer precursor solution comprises polydimethylsiloxane, a curing agent and a diluent;
(5) And stripping the glass substrate to obtain the double-layer thermal response photonic crystal film.
6. The method for preparing a two-layer thermal response photonic crystal thin film device according to claim 5, wherein in the step (4), the volume ratio of the polydimethylsiloxane, the curing agent and the diluent is 0.1-0.3.
7. The method of claim 5, wherein the vertical deposition solution has a concentration of 0.5-2wt% in step (1).
8. The method for preparing a double-layer thermal response photonic crystal thin film device according to claim 5, wherein in the step (2), the molar ratio of the color developing agent, the color masking agent and the solvent is 1-3:1-3.
9. The method for preparing a dual-layer thermal response photonic crystal thin film device according to claim 5, wherein in the step (2), the weight ratio of the thermochromic phase change system, the diluent polymer, the polydimethylsiloxane and the curing agent is 0.05-0.1.
10. The bilayer thermally responsive photonic crystal thin film device of claim 5, wherein said developer is a phenol, sulfonic acid, carboxylic acid and halohydrin and their derivatives; the leuco agent is one of triarylmethane, phenothiazine, fluorane, spiropyran or rhodamine B lactam; the solvent is alcohol, ether, ketone, phosphate, carboxylate, sulfonate, sulfite and the like, and the diluent is one of alcohol, hydrocarbon, ether or ketone.
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| CN116496501A (en) * | 2023-04-04 | 2023-07-28 | 浙江精一新材料科技有限公司 | Liquid polysiloxane with lactam group and light valve |
| CN116496501B (en) * | 2023-04-04 | 2024-03-29 | 浙江精一新材料科技有限公司 | Liquid polysiloxane with lactam group and light valve |
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