CN112778465A - Preparation method of reversible color-changing photonic crystal hydrogel film - Google Patents
Preparation method of reversible color-changing photonic crystal hydrogel film Download PDFInfo
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Abstract
The invention relates to a preparation method of a reversible color-changing photonic crystal hydrogel film. The method comprises the following steps: preparing a layer of uniform and bright photonic crystal film on a hydrophilic glass slide by vertical deposition self-assembly; uniformly mixing acrylamide, isopropyl acrylamide, polyethylene glycol diacrylate, N' -methylene diacrylamide and a photoinitiator in an organic solvent to obtain a mixed solution; and (3) taking the prepared photonic crystal film as a template, infiltrating the mixed solution into the gaps of the photonic crystal film by using a clamping piece method for filling, and initiating polymerization by ultraviolet light to obtain the photonic crystal hydrogel film. The method is simple to operate, does not need special equipment, and the obtained photonic hydrogel film has excellent mechanical tensile property, sensitive humidity responsiveness and organic solvent responsiveness, and can be applied to the fields of sensing, detection and the like.
Description
Technical Field
The invention relates to a preparation method of reversible color-changing hydrogel, in particular to a preparation method of photonic crystal hydrogel with humidity and organic solvent sensitivity and rapid reversible color change.
Background
The photonic crystal is an ordered structure material formed by periodically arranging two or more substances with different refractive indexes (dielectric constants), and a periodic structure formed by alternately arranging materials with high refractive indexes and low refractive indexes can generate a photonic crystal band gap (similar to a forbidden band in a semiconductor). The photonic crystal is mainly characterized in that the photonic band gap is adopted, when the band gap falls in a visible light range, light waves can be reflected and refracted for multiple times in the photonic crystal, the reflected light and the refracted light are mutually superposed to form Bragg diffraction, and macroscopically, the photonic crystal shows bright structural color.
The responsive photonic crystal is a combination of the photonic crystal and a stimulus responsive intelligent material, and the photonic band gap energy of the responsive photonic crystal is changed along with external stimulus. The principle is that under the stimulation of physical or chemical signals, the period or dielectric constant of the photonic crystal changes, and then the photonic band gap is changed. Polymer materials based on stimuli responsiveness undergo strong volume expansion or contraction upon changes in external conditions, such as pressure, pH, temperature, solvents, electric fields, magnetic fields, and the like.
The photonic crystal hydrogel is a combination of a photonic crystal and hydrogel, and is characterized in that the volume response behavior of responsive hydrogel is combined with the band gap of the photonic crystal, and the band gap structure is changed through the expansion and contraction of the gel, so that the color-changing sensing behavior is generated. At present, researchers have conducted extensive research on responsive photonic crystal hydrogel, and have proposed wide applications in the fields of temperature, humidity, pressure sensing, ion detection, color display, anti-counterfeiting and the like, but are limited to different degrees in response sensitivity, limited color change range, reusability and the like.
Disclosure of Invention
The invention mainly solves the technical problem of providing a preparation method of the photonic crystal hydrogel with humidity and solvent sensitivity and rapid reversible color change.
The technical scheme of the invention is as follows: a preparation method of reversible color-changing photonic crystal hydrogel comprises the following specific steps:
(1) preparing a photonic crystal film: diluting and uniformly mixing the poly (styrene-acrylic acid) colloid nanoparticle emulsion with deionized water, vertically inserting a glass slide subjected to hydrophilic modification treatment into a diluent, treating under the conditions of constant temperature and constant humidity, and preparing a glass slide template with a self-assembled opal structure photonic crystal after the diluent is completely volatilized;
(2) preparation of the pre-gel solution: uniformly stirring and mixing acrylamide, isopropyl acrylamide, polyethylene glycol diacrylate, N' -methylene diacrylamide and a photoinitiator in a solvent to obtain a pre-gel solution; wherein the mass ratio of the acrylamide monomer, the isopropyl acrylamide monomer, the polyethylene glycol diacrylate, the N, N' -methylene diacrylamide, the photoinitiator to the solvent is (0.4-0.6): (0.3-0.5): (0.1-0.2): (0.01-0.03): (0.01-0.03): 1;
(3) preparing a photonic crystal hydrogel film: covering a clean glass slide on the glass slide template with the self-assembled opal structure photonic crystal obtained in the step (1), separating the two glass slides, infiltrating the pre-gel solution prepared in the step (2) between the two glass slides by using capillary force, filling gaps among colloid particles in a photonic crystal film, and performing photopolymerization under an ultraviolet lamp;
(4) and (4) soaking the cured photonic crystal hydrogel film obtained in the step (3) in deionized water and ethanol for cleaning (1-3 times), and removing the residual organic liquid to obtain the reversible color-changing photonic crystal hydrogel.
Preferably, the preparation method of the poly (styrene-acrylic acid) colloidal nanoparticle emulsion described in the step (1) is described in the references Macromolecular Chemistry and physics, Vol.207(2006) pp.596-604; the particle size of the poly (styrene-acrylic acid) colloidal nano particles is 140 nm-180 nm.
Preferably, the glass-carrying sheet subjected to hydrophilic modification treatment in the step (1) is subjected to ultrasonic cleaning by using ethanol, dried and then placed in a sub-atmospheric pressure glow discharge treatment machine for surface hydrophilic modification.
Preferably, the mass ratio of the diluted poly (styrene-acrylic acid) colloidal nanoparticles to the deionized water in the step (1) is (0.001-0.003): 1; the constant temperature and humidity condition is that the temperature is 50-70 ℃ and the humidity is 60-90%.
Preferably, the solvent in step (2) is at least one of water or ethylene glycol.
Preferably, the photoinitiator in the step (2) is 2-hydroxy-2-methylphenylacetone or 2-hydroxy-4- (2-hydroxyethoxy) -2-methylphenylacetone.
Preferably, the distance between the two glass slides in the step (3) is 0.3-1 mm.
Preferably, the irradiation time of the photopolymerization under an ultraviolet lamp (the ultraviolet lamp is a 100W short arc mercury lamp) in the step (3) is 60-120 seconds.
The invention is implemented as follows: an opal photonic crystal film which is vertically deposited and self-assembled on a glass slide is taken as a template; uniformly mixing acrylamide, isopropyl acrylamide, polyethylene glycol diacrylate, N' -methylene diacrylamide and a photoinitiator in an organic solvent to obtain a pre-gel solution; initiating polymerization under ultraviolet light; fully soaking in deionized water to finally obtain the photonic crystal hydrogel which is sensitive to humidity and solvent and can rapidly change color reversibly.
Advantageous effects
(1) The preparation method is based on the poly (styrene-acrylic acid) colloidal nanoparticles with good monodispersity, combines the hydrogel preparation technology with the photonic crystal technology, and has simple and controllable operation and strong repeatability;
(2) the hydrogel prepared by the invention has excellent optical performance, bright structural color and good mechanical performance, and particularly can sensitively and rapidly present different color changes visible to naked eyes under the stimulation of different humidity and solvents;
(3) the invention does not need to adopt complex equipment and has reference application value in the aspects of humidity monitoring, organic solvent detection and the like.
Drawings
FIG. 1 is an electron micrograph of an opal photonic crystal layer according to example 1 of the present invention;
FIG. 2 is an electron microscope scan of a photonic crystal hydrogel film of example 1 of the present invention;
FIG. 3 is a graph of the color change of a photonic crystal hydrogel of example 1 of the present invention at different humidities;
FIG. 4 is a graph of normalized reflectance spectra of photonic crystal hydrogel of example 1 of the present invention at different humidities;
FIG. 5 is a graph of humidity cycle number versus diffraction wavelength for photonic crystal hydrogels of example 1 of the present invention;
FIG. 6 is a graph of the color change of the photonic crystal hydrogel of example 1 of the present invention in different solvents.
Detailed Description
Example 1
Immersing the glass slide into ethanol, ultrasonically cleaning for 30min, drying, and then putting into a sub-atmospheric pressure glow discharge processor for surface hydrophilic modification for 2min to obtain a surface hydrophilic modified glass slide; taking poly (styrene-acrylic acid) colloidal nanoparticle emulsion with the particle size of 160nm, diluting and uniformly mixing the poly (styrene-acrylic acid) colloidal nanoparticle emulsion and deionized water according to the mass ratio of 0.002:1 to obtain diluted dispersion liquid, placing the diluted dispersion liquid into a 50mL beaker, vertically and vertically inserting a hydrophilic modified glass slide into the beaker, fixing the glass slide, placing the glass slide into a constant temperature and humidity box (the temperature is 60 ℃ and the humidity is 80%) for self-assembly, and after the diluted dispersion liquid is completely volatilized, preparing a glass slide template with opal-structured photonic crystals, wherein the glass slide template shows a bright purple structural color;
performing electron microscope scanning on the photonic crystal film, and displaying the result as shown in figure 1, wherein the prepared photonic crystal film consists of monodisperse colloidal particles which are closely arranged in a short-range order;
adding 0.48g of acrylamide, 0.4g of isopropylacrylamide, 0.1g of polyethylene glycol diacrylate (weight average molecular weight 575), 0.01g N, N' -methylenebisacrylamide and 0.02g of 2-hydroxy-2-methylphenylacetone into 1g of ethylene glycol, and uniformly mixing to obtain a pre-gel solution;
covering a clean glass slide on the glass slide of the opal-structure photonic crystal assembled by 160nm poly (styrene-acrylic acid) colloidal nanoparticles, wherein the two glass slides are separated by 0.3mm, penetrating the prepared pre-gel solution between the two glass slides by using the capillary force and filling gaps among colloidal particles in the photonic crystal film, and performing photopolymerization for 60s under an ultraviolet lamp (an ultraviolet lamp is a 100W short-arc mercury lamp) to prepare the photonic hydrogel film;
and soaking the obtained cured photonic crystal hydrogel film in deionized water and absolute ethyl alcohol in sequence for cleaning, and removing the organic solution to obtain the photonic crystal hydrogel with humidity and solvent sensitivity and reversible color change.
The photonic crystal hydrogel structure is subjected to electron microscope scanning, and the result is shown in fig. 2, and the result shows that the hydrogel is completely filled in the gaps of the colloidal particles and does not influence the ordered structure of the colloidal particles.
The reversible color-changing photonic crystal hydrogel is placed in a closed glass cover, the humidity in the sealed glass cover is controlled by a humidity controller, and the photonic crystal hydrogel film can be observed to have obvious color change and continuous red shift along with the increase of the humidity, and the result is shown in fig. 3 and fig. 4. Fig. 3 is a color chart of the photonic crystal hydrogel provided by the embodiment of the present invention at 40% to 100% relative humidity, and fig. 4 is a normalized reflection spectrogram of the photonic crystal hydrogel provided by the embodiment of the present invention at 40% to 100% relative humidity. As can be seen from fig. 3 and 4, when the relative humidity reached 40%, a significant color change of the photonic crystal hydrogel film was observed. When the relative humidity is 40%, the reflection wavelength of the photonic crystal hydrogel is 477nm, and the photonic crystal hydrogel is purple; when the relative humidity is 50%, the reflection wavelength of the photonic crystal hydrogel is 490nm, and the photonic crystal hydrogel is blue; when the relative humidity is 60%, the reflection wavelength of the photonic crystal hydrogel is 520nm, and the photonic crystal hydrogel is green; when the relative humidity is 70%, the reflection wavelength of the photonic crystal hydrogel is 555nm, and the photonic crystal hydrogel is yellow green; when the relative humidity is 80%, the reflection wavelength of the photonic crystal hydrogel is 590nm, and the photonic crystal hydrogel is yellow; when the relative humidity is 90%, the reflection wavelength of the photonic crystal hydrogel is 630nm, and the photonic crystal hydrogel is orange-red; when the relative humidity is 100%, the reflection wavelength of the photonic crystal hydrogel is 650nm, and the photonic crystal hydrogel is red. Therefore, the reversible color-changing photonic crystal hydrogel provided by the invention can change color along with the change of humidity, can realize rapid and visual detection in the relative humidity range of 40-100%, and can be rapidly recovered to be nearly colorless and transparent within 5s when the relative humidity is lower than 40%.
The reversible color-changing photonic crystal hydrogel is repeatedly changed in a circulating mode in an environment with relative humidity of 50% and 100%, and the result is shown in fig. 5, and fig. 5 is a graph of the relationship between the circulating times and the diffraction wavelength of the photonic crystal hydrogel provided by the embodiment of the invention in the environment with relative humidity of 50% and 100%, respectively. As can be seen from FIG. 5, the color-changing photonic crystal hydrogel provided by the invention can be used repeatedly, and has good humidity reversible color change and repeated detection capabilities.
Example 2
Immersing the glass slide into ethanol, ultrasonically cleaning for 30min, drying, and then putting into a sub-atmospheric pressure glow discharge processor for surface hydrophilic modification to obtain a surface hydrophilic modified glass slide; taking a poly (styrene-acrylic acid) colloidal nanoparticle emulsion with the particle size of 180nm, diluting and uniformly mixing the poly (styrene-acrylic acid) colloidal nanoparticle emulsion and deionized water according to the mass ratio of 0.001:1 to obtain a dilute dispersion liquid, placing the dilute dispersion liquid into a 50mL beaker, vertically and vertically inserting a hydrophilic modified glass slide into the beaker, fixing the glass slide, placing the glass slide into a constant temperature and humidity box (the temperature is 50 ℃ and the humidity is 70%) for self-assembly, and after the dilute dispersion liquid is completely volatilized, preparing a glass slide template with an opal structure photonic crystal, wherein the glass slide template shows a bright blue structural color;
adding 0.4g of acrylamide, 0.3g of isopropylacrylamide, 0.15g of polyethylene glycol diacrylate (weight average molecular weight 575), 0.02g N, N' -methylenebisacrylamide and 0.01g of 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone into 1g of water, and uniformly mixing to obtain a pre-gel solution;
covering a clean glass slide on the glass slide of the opal-structure photonic crystal assembled by 180nm poly (styrene-acrylic acid) colloidal nanoparticles, wherein the distance between the two glass slides is 0.5mm, penetrating the prepared pre-gel solution between the two glass slides by using the capillary force and filling the gaps between colloidal particles in the photonic crystal film, and performing photopolymerization for 120s under an ultraviolet lamp (an ultraviolet lamp is a 100W short-arc mercury lamp) to prepare the photonic hydrogel film;
and (3) sequentially soaking the obtained cured photonic crystal hydrogel film in deionized water and absolute ethyl alcohol for cleaning for 2 times, and removing the organic solution to obtain the humidity and solvent sensitive reversible color-changing photonic crystal hydrogel.
The reversible color-changing photonic crystal hydrogel is placed in ethanol, methanol, dimethyl sulfoxide and water respectively, and the color change is observed, and the result is shown in figure 6. As can be seen in fig. 6, the photonic hydrogel appeared orange-red when placed in ethanol; when placed in methanol, the photonic hydrogel immediately changes color, appearing red; when placed in dimethyl sulfoxide, the color of the photonic hydrogel changes immediately, appearing purple; when placed in water, the photonic hydrogel immediately changes color, appearing pink.
Example 3
Immersing the glass slide into ethanol, ultrasonically cleaning for 30min, drying, and then putting into a sub-atmospheric pressure glow discharge processor for surface hydrophilic modification to obtain a surface hydrophilic modified glass slide; taking a poly (styrene-acrylic acid) colloidal nanoparticle emulsion with the particle size of 140nm, diluting and uniformly mixing the poly (styrene-acrylic acid) colloidal nanoparticle emulsion and deionized water according to the mass ratio of 0.003:1 to obtain a dilute dispersion liquid, placing the dilute dispersion liquid into a 50mL beaker, vertically and vertically inserting a hydrophilic modified glass slide into the beaker, fixing the glass slide, placing the glass slide into a constant temperature and humidity box (the temperature is 70 ℃ and the humidity is 90%) for self-assembly, and after the dilute dispersion liquid is completely volatilized, preparing a glass slide template with an opal-structure photonic crystal, wherein the glass slide template shows a bright blue structural color;
adding 0.6g of acrylamide, 0.5g of isopropylacrylamide, 0.2g of polyethylene glycol diacrylate (weight average molecular weight 575), 0.03g N, N' -methylenebisacrylamide and 0.03g of 2-hydroxy-2-methylphenylacetone into a mixed solvent of 0.8g of ethylene glycol and 0.2g of deionized water, and uniformly mixing to obtain a pre-gel solution;
covering a clean glass slide on the glass slide of the opal-structure photonic crystal assembled by 140nm poly (styrene-acrylic acid) colloidal nanoparticles, wherein the two glass slides are spaced by 1mm, penetrating the prepared pre-gel solution between the two glass slides by using capillary force and filling gaps among colloidal particles in the photonic crystal film, and performing photopolymerization for 80s under an ultraviolet lamp (the ultraviolet lamp is a 100W short-arc mercury lamp) to prepare the photonic hydrogel film;
and (3) sequentially soaking the obtained cured photonic crystal hydrogel film in deionized water and absolute ethyl alcohol for cleaning for 3 times, and removing the organic solution to obtain the humidity and solvent sensitive reversible color-changing photonic crystal hydrogel.
Claims (7)
1. The preparation method of the reversible color-changing photonic crystal hydrogel comprises the following specific steps:
(1) preparing a photonic crystal film: diluting and uniformly mixing the poly (styrene-acrylic acid) colloid nanoparticle emulsion with deionized water, vertically inserting a glass slide subjected to hydrophilic modification treatment into a diluent, treating under the conditions of constant temperature and constant humidity, and preparing a glass slide template with a self-assembled opal structure photonic crystal after the diluent is completely volatilized;
(2) preparation of the pre-gel solution: uniformly stirring and mixing acrylamide, isopropyl acrylamide, polyethylene glycol diacrylate, N' -methylene diacrylamide and a photoinitiator in a solvent to obtain a pre-gel solution; wherein the mass ratio of the acrylamide monomer, the isopropyl acrylamide monomer, the polyethylene glycol diacrylate, the N, N' -methylene diacrylamide, the photoinitiator to the solvent is (0.4-0.6): (0.3-0.5): (0.1-0.2): (0.01-0.03): (0.01-0.03): 1;
(3) preparing a photonic crystal hydrogel film: covering a clean glass slide on the glass slide template with the self-assembled opal structure photonic crystal obtained in the step (1), separating the two glass slides, infiltrating the pre-gel solution prepared in the step (2) between the two glass slides by using capillary force, filling gaps among colloid particles in a photonic crystal film, and performing photopolymerization under an ultraviolet lamp;
(4) and (4) cleaning the cured photonic crystal hydrogel film obtained in the step (3) to obtain the reversible color-changing photonic crystal hydrogel.
2. The method of claim 1, wherein: the particle size of the poly (styrene-acrylic acid) colloidal nanoparticles in the step (1) is 140 nm-180 nm.
3. The method of claim 1, wherein: the mass ratio of the diluted poly (styrene-acrylic acid) colloidal nanoparticles to the deionized water in the step (1) is (0.001-0.003): 1; the constant temperature and humidity condition is that the temperature is 50-70 ℃ and the humidity is 60-90%.
4. The method of claim 1, wherein: the solvent in the step (2) is at least one of water or ethylene glycol.
5. The method of claim 1, wherein: the photoinitiator in the step (2) is 2-hydroxy-2-methylphenyl acetone or 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl phenylpropanone.
6. The method of claim 1, wherein: the distance between the two glass slides in the step (3) is 0.3-1 mm.
7. The method of claim 1, wherein: and (4) the irradiation time of photopolymerization under an ultraviolet lamp in the step (3) is 60-120 seconds.
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| CN113625498A (en) * | 2021-08-13 | 2021-11-09 | 上海应用技术大学 | Preparation method of electric field controllable silicon dioxide colloid self-assembly structure color-changing device |
| CN114603759A (en) * | 2022-03-04 | 2022-06-10 | 北京航空航天大学 | Preparation method of crack-free photonic crystal |
| CN114752168A (en) * | 2022-03-31 | 2022-07-15 | 华南农业大学 | Angle-dependency-free structural color hydrogel film, and preparation method and application thereof |
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| CN106084123A (en) * | 2016-06-03 | 2016-11-09 | 江南大学 | A kind of can the counter opal gel photonic crystal sensing membrane of open hole detection concentration of cadmium ions |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113625498A (en) * | 2021-08-13 | 2021-11-09 | 上海应用技术大学 | Preparation method of electric field controllable silicon dioxide colloid self-assembly structure color-changing device |
| CN114603759A (en) * | 2022-03-04 | 2022-06-10 | 北京航空航天大学 | Preparation method of crack-free photonic crystal |
| CN114603759B (en) * | 2022-03-04 | 2023-04-07 | 北京航空航天大学 | Preparation method of crack-free photonic crystal |
| CN114752168A (en) * | 2022-03-31 | 2022-07-15 | 华南农业大学 | Angle-dependency-free structural color hydrogel film, and preparation method and application thereof |
| CN114752168B (en) * | 2022-03-31 | 2023-03-03 | 华南农业大学 | Structure color hydrogel film without angle dependence, preparation method and application thereof |
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