CN118549359A - Method for visually detecting iron ions by utilizing inverse opal polymer photonic crystal - Google Patents
Method for visually detecting iron ions by utilizing inverse opal polymer photonic crystal Download PDFInfo
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Abstract
The invention belongs to the technical field of iron ion detection, and relates to a method for visually detecting iron ions by utilizing inverse opal polymer photonic crystals, wherein inverse opal polymer photonic crystals are placed in a solution to be detected, and then hexamethylenediamine solution is added to form a mixed system; the mixed system is uniformly oscillated, and the detection of the solution to be detected is realized by judging the change of the structural color of the inverse opal polymer photonic crystal and the movement of the reflection peak thereof; the functional monomer adopted in the preparation of the inverse opal polymer photonic crystal is a compound containing carboxyl. After iron ions are added into the system, the hexamethylenediamine aqueous solution and the iron ions undergo a coordination reaction to form a coordination compound, so that the hydrolysis process of hexamethylenediamine is inhibited, and compared with the process of adding only hexamethylenediamine aqueous solution, the swelling and the change of lattice constant are reduced, and the red shift of reflection peaks is reduced, thereby realizing the visual detection of the iron ions.
Description
Technical Field
The invention belongs to the technical field of iron ion detection, and particularly relates to a method for visually detecting iron ions by utilizing inverse opal polymer photonic crystals.
Background
In recent years, the urban, industrial and agricultural activities have led to the development, processing and use of more and more metal resources. Iron ions are a common metal ion which is mainly present in industrial wastewater, and the uncontrolled discharge causes pollution to water resources and soil, thereby causing serious harm to environment and organisms. The iron ion content is too high, which can cause eutrophication of water body and promote the growth of algae and bacteria. Meanwhile, if a human is contacted with high-concentration iron ions for a long time, the iron ions can irritate skin and eyes, so that skin allergy, blepharitis and other symptoms are caused, in addition, the iron ions can also have adverse effects on respiratory systems, nerves, digestive systems and other systems, and even serious diseases such as cancers can be caused when serious diseases are caused. Iron ion is one of the indispensable metal ions in life systems, and plays an important role in many physiological processes such as oxygen transportation and storage, electron transfer, enzyme catalysis, and the like. However, excessive iron ions can lead to liver damage, renal failure and even death.
Therefore, rapid, sensitive and reliable detection of iron ions is of great importance for the prevention of various health risks. In recent years, analysis technology and detection methods for iron ions are endless, such as electrochemical methods, liquid chromatography, atomic spectroscopy, spectrophotometry, fluorescence sensor methods and the like, and the methods have the problems of long time consumption, high cost, complicated instrument or synthesis process, complex operation and the like.
Disclosure of Invention
The invention aims to provide a method for visually detecting iron ions by utilizing inverse opal polymer photonic crystals, which solves the problems of long detection period, complex and tedious operation, high cost and the like in the existing method for detecting iron ions.
The invention is realized by the following technical scheme:
The invention discloses a method for visually detecting iron ions by utilizing inverse opal polymer photonic crystals, which comprises the following steps of:
Placing the inverse opal polymer photonic crystal in a solution to be detected, and then adding a hexamethylenediamine solution to form a mixed system;
the mixed system is uniformly oscillated, and the detection of the solution to be detected is realized by judging the change of the structural color of the inverse opal polymer photonic crystal and the movement of the reflection peak thereof;
The functional monomer adopted in the preparation of the inverse opal polymer photonic crystal is a compound containing carboxyl.
Further, the preparation method of the inverse opal polymer photonic crystal comprises the following steps:
Step one, carrying out ultrasonic mixing on SiO 2 particle suspension to obtain SiO 2 dispersion;
Step two, forming a photonic crystal film by a self-assembly method through SiO 2 dispersion liquid;
Step three, mixing a functional monomer, a cross-linking agent and an initiator in a solvent to form a copolymer system, and carrying out ultrasonic treatment to uniformly mix the copolymer system to obtain a precursor solution;
And fourthly, dropwise adding the precursor solution on the photonic crystal film for a plurality of times to uniformly fill the photonic crystal film in the gaps, polymerizing under an ultraviolet lamp, and etching after the polymerization is completed to obtain the inverse opal polymer photonic crystal.
Further, in the first step, siO 2 particles are solid or hollow silica particles with the particle size in the range of 150-450 nm;
the solvent used for ultrasonic mixing is ethanol, water or a mixture of the two.
Further, in the second step, the self-assembly method is vertical deposition, spray coating or spin coating.
Further, in the third step, the carboxyl group-containing compound is acrylic acid, methacrylic acid or itaconic acid.
In the third step, the cross-linking agent is ethylene glycol dimethacrylate;
the initiator is a photoinitiator or a thermal initiator;
The solvent is absolute ethanol, glycol or deionized water.
Further, in the third step, in the precursor solution, the molar ratio of the functional monomer to the crosslinking agent is 5: (0.01-2).
In the fourth step, the preparation process of the inverse opal polymer photonic crystal specifically comprises the following steps:
Placing the photonic crystal film in a culture dish with an inclined angle, and dripping a precursor solution to the surface of the photonic crystal film a small amount of times to enable the precursor solution to permeate into gaps of the photonic crystal film;
Covering the organic glass sheet soaked by ethanol on a photonic crystal film with a precursor solution on the surface, so that the organic glass sheet, the precursor solution and the photonic crystal film form a sandwich structure, and then placing the organic glass sheet, the precursor solution and the photonic crystal film under an ultraviolet lamp for irradiation to realize photopolymerization and solidification;
And (3) adding a proper amount of hydrofluoric acid solution into a culture dish with a sandwich structure after photopolymerization and solidification, etching silicon dioxide in the photonic crystal film, repeatedly flushing with deionized water after separation, and obtaining the inverse opal polymer photonic crystal after swelling balance and neutrality are achieved.
Further, the solution to be measured is an iron ion solution with the concentration of 1-1000 mu M and a ferrous ion solution with the concentration of 10-1000 mu M.
Further, hexamethylenediamine is contained in the mixed system at a concentration of 9 to 11mM.
Compared with the prior art, the invention has the following beneficial technical effects:
The invention discloses a method for visually detecting iron ions by utilizing an inverse opal polymer photonic crystal, when no iron ions exist in a mixed system, amino groups in hexamethylenediamine can accept hydrogen ions in water to form protonated amino groups, hydroxide ions are released, so that the solution is alkaline, the inverse opal polymer photonic crystal is swelled, the lattice constant is changed, and the reflection peak of the inverse opal polymer photonic crystal is red shifted; after iron ions are added into the system, the hexamethylenediamine aqueous solution and the iron ions undergo a coordination reaction to form a coordination compound, so that the hydrolysis process of hexamethylenediamine is inhibited, and compared with the process of adding only hexamethylenediamine aqueous solution, the swelling and the change of lattice constant are reduced, and the red shift of reflection peaks is reduced, thereby realizing the visual detection of the iron ions. Meanwhile, the iron ions and the ferrous ions can be distinguished according to the color of the generated complex. Compared with the traditional detection method, the method has the advantages of simple operation, high response speed, high sensitivity and low preparation cost, and can realize on-site real-time visual detection without special operation or large-scale instrument, and has response to iron ions with the concentration of 1-1000 mu M and ferrous ions with the concentration of 10-1000 mu M.
Further, the preparation process of the inverse opal polymer photonic crystal of the invention specifically comprises the following steps: preparing a precursor solution containing a functional monomer, a cross-linking agent and an initiator, then penetrating the obtained precursor solution into a photonic crystal film, covering an organic glass sheet on the precursor solution, irradiating the organic glass sheet under an ultraviolet lamp to perform polymerization reaction, etching the organic glass sheet by hydrofluoric acid after polymerization is completed, and transferring the polymer photonic crystal with responsiveness onto the organic glass sheet to obtain the inverse opal polymer photonic crystal. As the functional monomer is a compound containing carboxyl, the surface of the inverse opal polymeric photonic crystal contains a large amount of carboxyl, the solution is alkaline when hexamethylenediamine is hydrolyzed, and the carboxyl is dissociated in the alkaline solution, so that the inverse opal polymeric photonic crystal absorbs water and swells.
Drawings
FIG. 1 is a graph of reflectance spectra of an inverse opal polymer photonic crystal sensor of example 1 when detecting deionized water;
FIG. 2 is a reflectance spectrum of the inverse opal polymer photonic crystal sensor of example 2 for detecting 1. Mu.M iron ions;
FIG. 3 is a reflectance spectrum of the inverse opal polymer photonic crystal sensor of example 3 for detecting 10. Mu.M iron ions;
FIG. 4 is a reflectance spectrum of the inverse opal polymer photonic crystal sensor of example 4 for detecting 100. Mu.M iron ions;
FIG. 5 is a reflectance spectrum of the inverse opal polymer photonic crystal sensor of example 5 for detecting 1000. Mu.M iron ions;
FIG. 6 is a reflectance spectrum of the inverse opal polymer photonic crystal sensor of example 6 for detecting 10. Mu.M ferrous ions;
FIG. 7 is a reflectance spectrum of the inverse opal polymer photonic crystal sensor of example 7 for detecting 50. Mu.M ferrous ions;
FIG. 8 is a reflectance spectrum of the inverse opal polymer photonic crystal sensor of example 8 for detecting 100. Mu.M ferrous ions;
FIG. 9 is a reflectance spectrum of the inverse opal polymer photonic crystal sensor of example 9 for detecting 500. Mu.M ferrous ions;
FIG. 10 is a reflectance spectrum of the inverse opal polymer photonic crystal sensor of example 10 for detecting 1000. Mu.M ferrous ions;
FIG. 11 is a reflectance spectrum of an inverse opal polymer photonic crystal sensor of example 11 for detecting 100. Mu.M iron ions;
FIG. 12 is a reflectance spectrum of the inverse opal polymer photonic crystal sensor of example 12 for detecting 100. Mu.M ferrous ions added to an interfering solution;
FIG. 13 is a graph showing the reflectance spectrum of an inverse opal polymer photonic crystal sensor of example 13 with the addition of 9mM hexamethylenediamine to detect 10. Mu.M iron ions;
FIG. 14 is a reflectance spectrum of an inverse opal polymer photonic crystal sensor of example 14 with the addition of 9mM hexamethylenediamine to detect 10. Mu.M ferrous ions;
FIG. 15 is a graph showing the reflectance spectrum of an inverse opal polymer photonic crystal sensor of example 15 with the addition of 11mM hexamethylenediamine to detect 10. Mu.M iron ions;
FIG. 16 is a graph showing the reflectance spectrum of an inverse opal polymer photonic crystal sensor of example 16 with the addition of 11mM hexamethylenediamine to detect 10. Mu.M ferrous ions.
Detailed Description
The objects, technical solutions and advantages of the present invention will be more apparent from the following detailed description with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention, i.e., the embodiments described are only some, but not all, of the embodiments of the invention.
The components illustrated in the figures and described and shown in the embodiments of the invention may be arranged and designed in a wide variety of different configurations, and thus the detailed description of the embodiments of the invention provided in the figures below is not intended to limit the scope of the invention as claimed, but is merely representative of selected ones of the embodiments of the invention. All other embodiments, which can be made by a person skilled in the art without making any inventive effort, are intended to be within the scope of the present invention, based on the figures and embodiments of the present invention.
It should be noted that: the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, element, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, element, method, article, or apparatus. The features and properties of the present invention are described in further detail below with reference to examples.
The invention aims to provide a method for detecting iron ions by using a photonic crystal in a visual way. The method comprises the following specific steps:
step one: the prepared SiO 2 granule suspension is prepared into a dispersion with the concentration of 0.3 to 1 weight percent, and is mixed for 1 to 3 hours by ultrasonic treatment for standby.
Step two: and forming a photonic crystal film on the glass sheet by using the ultrasonic uniform dispersion liquid through a self-assembly method.
Step three: the functional monomer, the cross-linking agent and the initiator are mixed in a solvent according to a certain proportion to form a copolymer system, and the copolymer system is subjected to ultrasonic treatment to be uniformly mixed to obtain a precursor solution, and the precursor solution is refrigerated for standby.
Step four: and placing the prepared photonic crystal film in a glass culture dish with an inclination angle of 10 degrees, and dripping precursor solution into the bottom of the photonic crystal film for a plurality of times to ensure that the solution is uniformly filled in gaps of SiO 2 particles by means of gravity and capillary force. Covering an organic glass sheet which is rinsed by ethanol on a photonic crystal film containing a precursor solution, enabling the organic glass sheet, the precursor solution and the glass sheet to be in a sandwich structure, wiping redundant liquid at the edge of the sandwich structure by using filter paper after pinching by tweezers, putting the redundant liquid into a culture dish again, and performing polymerization curing for 3 hours under ultraviolet and the like.
After solidification, the constructed sandwich structure is moved to a plastic culture dish, hydrofluoric acid solution with volume concentration of 4% is added into the sandwich structure, silicon dioxide in the photonic crystal film is etched, and after the organic and glass sheets are separated, the inverse opal polymer photonic crystal is displayed on one side of the organic glass. And repeatedly flushing the inverse opal polymer photonic crystal by using deionized water to ensure that the inverse opal polymer photonic crystal reaches swelling balance and is neutral, and then soaking the inverse opal polymer photonic crystal in deionized water for standby.
Step five: placing the prepared inverse opal polymer photonic crystal into a solution to be detected to obtain a complete inverse opal polymer photonic crystal sensor system;
Step six: and adding hexamethylenediamine solution to obtain a mixed system, oscillating uniformly, and detecting the solution to be detected by observing the change of the structural color of the inverse opal polymer photonic crystal and the movement of the reflection peak of the inverse opal polymer photonic crystal.
In the first step: the adopted solid SiO 2 particles with the concentration of 0.5 weight percent are 210nm, and the solvent is ethanol.
In the second step: a photonic crystal film is prepared by adopting a vertical deposition method.
In the third step: the molar ratio of the functional monomer to the cross-linking agent is 5 (0.1-2), the solvent is 1mL, the initiator is 20 mu L, wherein the functional monomer is acrylic acid, the cross-linking agent is ethylene glycol dimethacrylate, the initiator is photoinitiator (2-hydroxy-2-methyl propiophenone), and the solvent is absolute ethyl alcohol.
In the fifth step, the solution to be measured is iron ion with the concentration of 1-1000 mu M, ferrous ion with the concentration of 10-1000 mu M or deionized water.
In the sixth step, the concentration of hexamethylenediamine in the mixed system is 9-11mM.
The essence of photonic crystals is that the propagation of light is selectively hindered or limited by the periodic arrangement of two or more materials of different refractive index. The sensor constructed by the method is widely applied to the fields of biology and chemistry, can show reflection peaks or macroscopic structural color changes after encountering specific stimulus, and has the advantage of visual and visible detection results. The inverse opal polymer photonic crystal sensor prepared by the sacrificial template method has the advantages of good flexibility, large specific surface area, high porosity and the like, and has high response rate when analyzing the object to be detected. According to the invention, iron ions are introduced into the inverse opal polymer photonic crystal responding to hexamethylenediamine, and a novel method for detecting the iron ions is explored to meet detection requirements of simplicity in operation, quick response time, visual and visible results, low price and the like.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 1 hour for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and then the mixture is refrigerated for standby.
Step four: and placing the prepared photonic crystal film in a glass culture dish with an inclination angle of 10 degrees, and dripping precursor solution into the bottom of the photonic crystal film for a plurality of times to ensure that the solution is uniformly filled in gaps of SiO 2 particles by means of gravity and capillary force. Covering an organic glass sheet which is rinsed by ethanol on a photonic crystal film containing a precursor solution, enabling the organic glass sheet, the precursor solution and the glass sheet to be in a sandwich structure, wiping redundant liquid at the edge of the sandwich structure by using filter paper after pinching by tweezers, putting the redundant liquid into a culture dish again, and performing polymerization curing for 3 hours under ultraviolet and the like.
After solidification, the constructed sandwich structure is moved to a plastic culture dish, hydrofluoric acid solution with volume concentration of 4% is added into the sandwich structure, silicon dioxide in the photonic crystal film is etched, and after the organic and glass sheets are separated, the inverse opal polymer photonic crystal is displayed on one side of the organic glass. And repeatedly flushing the inverse opal polymer photonic crystal by using deionized water to ensure that the inverse opal polymer photonic crystal reaches swelling balance and is neutral, and then soaking the inverse opal polymer photonic crystal in deionized water for standby.
During detection, the inverse opal polymer photonic crystal is put into 9mL of deionized water; 1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the detection concentration of the prepared inverse opal polymer photonic crystal is 10mM hexamethylenediamine, the inverse opal polymer photonic crystal swells due to the hydrolysis of the hexamethylenediamine solution, and the reflection peak of the inverse opal polymer photonic crystal is red shifted. As can be seen from FIG. 1, when only 10mM hexamethylenediamine was contained in the system, the reflection peak was red-shifted from 485nm to 692nm by 207nm, and the structural color was changed from blue to red. According to the reflection peak of the inverse opal polymer photonic crystal and the structural color exhibited by the inverse opal polymer photonic crystal.
Example 2
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 1 hour for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and then the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for detecting 1 μm iron ion solution was as follows:
the inverse opal polymer photonic crystal was placed in 1mL of a mixed solution of 10 μm ferric ion solution and 8mL of deionized water;
1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the prepared inverse opal polymer photonic crystal detects iron ion solution with the concentration of 1 mu M, as the hexamethylenediamine aqueous solution and the iron ion undergo a coordination reaction to form a coordination compound, the hydrolysis process of the hexamethylenediamine is inhibited, and compared with the process of adding only hexamethylenediamine aqueous solution, the swelling and the change of lattice constant of the inverse opal polymer photonic crystal are reduced, and the red shift of reflection peaks is reduced, so that the visual detection of the iron ion is realized. As can be seen from fig. 1 and 2, when only 10mM hexamethylenediamine is contained in the system, the reflection peak is red-shifted from 485nm to 692nm by 207nm, and the structural color is changed from blue to red; when the system contains 1 mu M of iron ions and 10mM of hexamethylenediamine, the reflection peak is red-shifted from 485nm to 682nm, the red-shift amount is 197nm, and the structural color is changed from blue to red. According to the reflection peak of the inverse opal polymer photonic crystal and the structural color presented by the reflection peak, the visual detection of 1 mu M iron ions is realized.
Example 3
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 1 hour for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and then the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for detecting 10 μm iron ion solution was as follows:
the inverse opal polymer photonic crystal was placed in 1mL of a mixed solution of 100 μm ferric ion solution and 8mL of deionized water;
1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the prepared inverse opal polymer photonic crystal detects iron ion solution with the concentration of 10 mu M, as the hexamethylenediamine aqueous solution and the iron ion undergo a coordination reaction to form a coordination compound, the hydrolysis process of the hexamethylenediamine is inhibited, and compared with the process of adding only hexamethylenediamine aqueous solution, the swelling and the change of lattice constant of the inverse opal polymer photonic crystal are reduced, and the red shift of reflection peaks is reduced, so that the visual detection of the iron ion is realized. As can be seen from fig. 1 and 3, when the system contains only 10mM hexamethylenediamine solution, the reflection peak is red-shifted from 485nm to 692nm by 207nm, and the structural color is changed from blue to red; when the system contains 10 mu M of iron ions and 10mM of hexamethylenediamine, the reflection peak is red-shifted from 485nm to 615nm, the red-shift amount is 130nm, and the structural color is changed from blue to orange. According to the reflection peak of the inverse opal polymer photonic crystal and the structural color presented by the reflection peak, the visual detection of 10 mu M iron ions is realized.
Example 4
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 1 hour for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.01, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and then the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for detecting 100 μm iron ion solution was as follows:
placing the inverse opal polymer photonic crystal into 1mL of a mixed solution of 1000 mu M ferric ion solution and 8mL of deionized water;
1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the detection concentration of the prepared inverse opal polymer photonic crystal is 100 mu M of iron ion solution, as the hexamethylenediamine aqueous solution and the iron ion undergo a coordination reaction to form a coordination compound, the hydrolysis process of the hexamethylenediamine is inhibited, and compared with the process of adding only the hexamethylenediamine aqueous solution, the swelling and the change of the lattice constant of the inverse opal polymer photonic crystal are reduced, and the red shift of the reflection peak is reduced, so that the visual detection of the iron ion is realized. As can be seen from fig. 1 and 4, when only 10mM hexamethylenediamine is contained in the system, the reflection peak is red-shifted from 485nm to 692nm by 207nm, and the structural color is changed from blue to red; when the system contains 100 mu M iron ions and 10mM hexamethylenediamine, the reflection peak is red-shifted from 485nm to 556nm and the red-shift amount is 71nm, and the structural color is changed from blue to green. According to the reflection peak of the inverse opal polymer photonic crystal and the structural color presented by the reflection peak, the visual detection of 100 mu M iron ions is realized.
Example 5
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 1 hour for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to a molar ratio of 5:2, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylacetone are added as photoinitiators to obtain a precursor solution required by experiments, and the precursor solution is fully mixed by ultrasonic treatment for 30min and then refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for detecting 1000 μm iron ion solution is as follows:
Placing the inverse opal polymer photonic crystal into 1mL of a mixed solution of 10000 mu M ferric ion solution and 8mL of deionized water;
1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the prepared inverse opal polymer photonic crystal detects iron ion solution with the concentration of 1000 mu M, as the hexamethylenediamine aqueous solution and the iron ion undergo a coordination reaction to form a coordination compound, the hydrolysis process of the hexamethylenediamine is inhibited, and compared with the process of adding only hexamethylenediamine aqueous solution, the swelling and the change of lattice constant of the inverse opal polymer photonic crystal are reduced, and the red shift of reflection peaks is reduced, so that the visual detection of the iron ion is realized. As can be seen from fig. 1 and 5, when only 10mM hexamethylenediamine is contained in the system, the reflection peak is red-shifted from 485nm to 692nm by 207nm, and the structural color is changed from blue to red; when the system contains 1000 mu M of iron ions and 10mM of hexamethylenediamine, the reflection peak is red-shifted from 485nm to 503nm, the red-shift amount is 18nm, and the structural color is changed from blue to blue-green. According to the reflection peak of the inverse opal polymer photonic crystal and the structural color presented by the reflection peak, the visual detection of 1000 mu M iron ions is realized.
Example 6
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 2 hours for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for detecting 10 μm ferrous ion solution was as follows:
placing the inverse opal polymer photonic crystal into 1mL of a mixed solution of 100 mu M ferrous ion solution and 8mL of deionized water;
1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the prepared inverse opal polymer photonic crystal is used for detecting ferrous ion solution with the concentration of 10 mu M, as the hexamethylenediamine aqueous solution and the ferrous ion undergo a coordination reaction to form a coordination compound, the hydrolysis process of the hexamethylenediamine is inhibited, and compared with the process of adding only hexamethylenediamine aqueous solution, the swelling and the change of lattice constant of the inverse opal polymer photonic crystal are reduced, and the red shift of reflection peaks is reduced, so that the visual detection of the ferrous ion is realized. As can be seen from fig. 1 and 6, when only 10mM hexamethylenediamine is contained in the system, the reflection peak is red-shifted from 485nm to 692nm by 207nm, and the structural color is changed from blue to red; when the system contains 10 mu M ferrous ion and 10mM hexamethylenediamine, the reflection peak is red-shifted from 485nm to 677nm, the red-shift amount is 192nm, and the structural color is changed from blue to red. According to the reflection peak of the inverse opal polymer photonic crystal and the structural color presented by the reflection peak, the visual detection of 10 mu M ferrous ions is realized.
Example 7
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is mixed for 3 hours by ultrasonic treatment for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for detecting 50 μm ferrous ion solution was as follows:
placing the inverse opal polymer photonic crystal into 5mL of a mixed solution of 500 mu M ferrous ion solution and 4mL of deionized water;
1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the prepared inverse opal polymer photonic crystal is used for detecting ferrous ion solution with the concentration of 50 mu M, as the hexamethylenediamine aqueous solution and the ferrous ion undergo a coordination reaction to form a coordination compound, the hydrolysis process of the hexamethylenediamine is inhibited, and compared with the process of adding only hexamethylenediamine aqueous solution, the swelling and the change of lattice constant of the inverse opal polymer photonic crystal are reduced, and the red shift of reflection peaks is reduced, so that the visual detection of the ferrous ion is realized. As can be seen from fig. 1 and 7, when only 10mM hexamethylenediamine is contained in the system, the reflection peak is red-shifted from 485nm to 692nm by 207nm, and the structural color is changed from blue to red; when the system contains 50 mu M ferrous ion and 10mM hexamethylenediamine, the reflection peak is red-shifted from 485nm to 640nm, the red-shift amount is 155nm, and the structural color is changed from blue to orange. According to the reflection peak of the inverse opal polymer photonic crystal and the structural color presented by the reflection peak, the visual detection of 50 mu M ferrous ions is realized.
Example 8
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is mixed for 3 hours by ultrasonic treatment for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for detecting 100 μm ferrous ion solution was as follows:
placing the inverse opal polymer photonic crystal into 1mL of a mixed solution of 1000 mu M ferrous ion solution and 8mL of deionized water;
1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the detection concentration of the prepared inverse opal polymer photonic crystal is 100 mu M ferrous ion solution, as the hexamethylenediamine aqueous solution and ferrous ion undergo a coordination reaction to form a coordination compound, the hydrolysis process of hexamethylenediamine is inhibited, and compared with the process of adding only hexamethylenediamine aqueous solution, the swelling and the change of lattice constant of the inverse opal polymer photonic crystal are reduced, and the red shift of reflection peaks is reduced, so that the visual detection of ferrous ion is realized. As can be seen from fig. 1 and 8, when only 10mM hexamethylenediamine is contained in the system, the reflection peak is red-shifted from 485nm to 692nm by 207nm, and the structural color is changed from blue to red; when the system contains 100 mu M ferrous ion and 10mM hexamethylenediamine, the reflection peak is red-shifted from 485nm to 588nm, the red-shift amount is 103nm, and the structural color is changed from blue to yellow-green. According to the reflection peak of the inverse opal polymer photonic crystal and the structural color presented by the reflection peak, the visual detection of 100 mu M ferrous ions is realized.
Example 9
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 1 hour for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for detecting 500 μm ferrous ion solution was as follows:
Placing the inverse opal polymer photonic crystal into 5mL of a mixed solution of 5000 mu M ferrous ion solution and 4mL of deionized water;
1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the prepared inverse opal polymer photonic crystal detects ferrous ion solution with the concentration of 500 mu M, because the hexamethylenediamine aqueous solution and the ferrous ion undergo a coordination reaction to form a coordination compound, the hydrolysis process of the hexamethylenediamine is inhibited, and compared with the process of adding only hexamethylenediamine aqueous solution, the swelling and the change of lattice constant of the inverse opal polymer photonic crystal are reduced, and the red shift of reflection peaks is reduced, so that the visual detection of the ferrous ion is realized. As can be seen from fig. 1 and 9, when only 10mM hexamethylenediamine is contained in the system, the reflection peak is red-shifted from 485nm to 692nm by 207nm, and the structural color is changed from blue to red; when the system contains 500 mu M ferrous ion and 10mM hexamethylenediamine, the reflection peak is red-shifted from 485nm to 541nm, the red-shift amount is 56nm, and the structural color is changed from blue to green. According to the reflection peak of the inverse opal polymer photonic crystal and the structural color presented by the reflection peak, the visual detection of 500 mu M ferrous ions is realized.
Example 10
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 2 hours for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for detecting 1000 μm ferrous ion solution was as follows:
Placing the inverse opal polymer photonic crystal into 1mL of a mixed solution of 10000 mu M ferrous ion solution and 8mL of deionized water;
1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the prepared inverse opal polymer photonic crystal detects ferrous ion solution with the concentration of 1000 mu M, because the hexamethylenediamine aqueous solution and the ferrous ion undergo a coordination reaction to form a coordination compound, the hydrolysis process of the hexamethylenediamine is inhibited, compared with the process of adding only hexamethylenediamine aqueous solution, the swelling and the change of lattice constant of the inverse opal polymer photonic crystal are reduced, and the red shift of reflection peaks is reduced, so that the visual detection of the ferrous ion is realized. As can be seen from fig. 1 and 10, when only 10mM hexamethylenediamine is contained in the system, the reflection peak is red-shifted from 485nm to 692nm by 207nm, and the structural color is changed from blue to red; when the system contains 1000 mu M of ferrous ion liquid and 10mM of hexamethylenediamine, the reflection peak is red-shifted from 485nm to 496nm, the red-shift amount is 11nm, and the structural color is changed from blue to blue-green. According to the reflection peak of the inverse opal polymer photonic crystal and the structural color presented by the reflection peak, the visual detection of 1000 mu M ferrous ions is realized.
Example 11
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is mixed for 3 hours by ultrasonic treatment for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for detecting a mixed solution of 100. Mu.M iron ions and 100. Mu.M interfering ions was as follows:
The inverse opal polymer photonic crystal was placed in a mixed solution of 1mL 1000. Mu.M ferric ion solution, 1mL 1000. Mu.M interfering ion, and 7mL deionized water;
1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the prepared inverse opal polymer photonic crystal detects the mixed solution of iron ions with the concentration of 100 mu M and interfering ions with the concentration of 100 mu M, as can be observed from fig. 11, after the interfering ion solution is added into the system, no obvious change is found in the reflection peak and the structural color, which indicates that the prepared inverse opal polymer photonic crystal has good anti-interference performance when detecting the iron ions.
Example 12
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 1 hour for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for detecting a mixed solution of 100. Mu.M ferrous ions and 100. Mu.M interfering ions was as follows:
Placing the inverse opal polymer photonic crystal into a mixed solution of 1mL of 1000 μM ferrous ion solution, 1mL of 1000 μM interfering ions and 7mL of deionized water;
1mL of 100mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the prepared inverse opal polymer photonic crystal detects the mixed solution of the ferrous ions with the concentration of 100 mu M and the interfering ions with the concentration of 100 mu M, as can be observed from fig. 12, after the interfering ion solution is added into the system, no obvious change is found in the reflection peak and the structural color, which indicates that the prepared inverse opal polymer photonic crystal has good anti-interference performance when the ferrous ions are detected.
Example 13
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 1 hour for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and then the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for the detection of 10 μm iron ion solution with the addition of hexamethylenediamine solution is as follows:
the inverse opal polymer photonic crystal was placed in 1mL of a mixed solution of 100 μm ferric ion solution and 8mL of deionized water;
1mL of 90mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when the 9mM hexamethylenediamine is added into the prepared inverse opal polymer photonic crystal sensor for detecting the iron ion solution with the concentration of 10 mu M, as the hexamethylenediamine aqueous solution and the iron ion undergo a coordination reaction to form a coordination compound, the hydrolysis process of the hexamethylenediamine is inhibited, and compared with the process of adding only the hexamethylenediamine aqueous solution, the swelling and the change of the lattice constant of the inverse opal polymer photonic crystal are reduced, the red shift of the reflection peak is reduced, so that the visual detection of the iron ion is realized. As compared with example 3, it can be seen from FIG. 13 that when the system contains 10. Mu.M of iron ion solution and 9mM of hexamethylenediamine solution, the reflection peak is red shifted from 485nm to 594nm by 109nm, and the structural color is changed from blue to yellowish green.
Example 14
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 2 hours for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and the mixture is refrigerated for standby.
Step four: the same as in example 1.
The procedure for the detection of 10. Mu.M ferrous ion solution by adding hexamethylenediamine solution was as follows:
placing the inverse opal polymer photonic crystal into 1mL of a mixed solution of 100 mu M ferrous ion solution and 8mL of deionized water;
1mL of 90mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: when 9mM hexamethylenediamine is added into the prepared inverse opal polymer photonic crystal, the detection concentration of which is 10 mu M ferrous ion solution, because the hexamethylenediamine aqueous solution and ferrous ion undergo a coordination reaction to form a coordination compound, the hydrolysis process of hexamethylenediamine is inhibited, and compared with the process of adding only hexamethylenediamine aqueous solution, the swelling and the change of lattice constant of the inverse opal polymer photonic crystal are reduced, and the red shift of reflection peaks is reduced, so that the visual detection of ferrous ions is realized. As compared with example 6, it can be seen from FIG. 14 that when the system contains 10. Mu.M ferrous ion solution and 9mM hexamethylenediamine, the reflection peak is red-shifted from 485nm to 640nm by 155nm, and the structural color is changed from blue to red.
Example 15
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
Step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 1 hour for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and the mixture is refrigerated for standby.
Step four: the same as in example 1.
The experimental procedure for the detection of 10 μm iron ion solution with the addition of hexamethylenediamine solution is as follows:
the inverse opal polymer photonic crystal was placed in 1mL of a mixed solution of 100 μm ferric ion solution and 8mL of deionized water;
1mL of 110mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: as compared with example 3, it can be seen from FIG. 15 that when an iron ion solution having a detection concentration of 10. Mu.M was added to the prepared inverse opal polymer photonic crystal sensor, the inverse opal polymer photonic crystal sensor swelled and broken due to the excessive basicity of the solution, and an irreversible change was generated with the disappearance of structural color and reflection peak.
Example 16
The preparation method of the inverse opal polymer photonic crystal comprises the following specific steps:
step one: the prepared SiO 2 granule suspension with the particle size of 210nm is prepared into a dispersion with the concentration of 0.5 weight percent, and is subjected to ultrasonic mixing for 2 hours for standby.
Step two: and self-assembling the ultrasonic uniform dispersion liquid on a glass sheet by a vertical deposition method to form the photonic crystal film.
Step three: acrylic acid is used as a functional monomer, ethylene glycol dimethacrylate is used as a cross-linking agent, a solution is prepared according to the molar ratio of 5:0.1, 1mL of absolute ethyl alcohol and 20 mu L of dihydroxydimethylbenzene acetone are added as photoinitiators to obtain a precursor solution required by experiments, the precursor solution is fully mixed by ultrasonic treatment for 30min, and the mixture is refrigerated for standby.
Step four: the same as in example 1.
The procedure for the detection of 10. Mu.M ferrous ion solution by adding hexamethylenediamine solution was as follows:
placing the inverse opal polymer photonic crystal into 1mL of a mixed solution of 100 mu M ferrous ion solution and 8mL of deionized water;
1mL of 110mM hexamethylenediamine solution is added, shaking is carried out uniformly, the color change of the film is observed, and the movement of the reflection peak of the photonic crystal is recorded, so that the detection of the solution to be detected is realized.
Conclusion: as compared with example 6, it can be seen from FIG. 16 that when 11mM hexamethylenediamine is added to the prepared inverse opal polymer photonic crystal sensor to detect a ferrous ion solution having a concentration of 10. Mu.M, the inverse opal polymer photonic crystal sensor swells and breaks due to the excessive basicity of the solution, causing irreversible changes accompanied by disappearance of structural color and reflection peak.
Finally, it should be noted that: the above embodiments are only for illustrating the technical aspects of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the above embodiments, it should be understood by those of ordinary skill in the art that: modifications and equivalents may be made to the specific embodiments of the invention without departing from the spirit and scope of the invention, which is intended to be covered by the claims.
Claims (10)
1. A method for visually detecting iron ions by using inverse opal polymer photonic crystals, which is characterized by comprising the following steps:
Placing the inverse opal polymer photonic crystal in a solution to be detected, and then adding a hexamethylenediamine solution to form a mixed system;
the mixed system is uniformly oscillated, and the detection of the solution to be detected is realized by judging the change of the structural color of the inverse opal polymer photonic crystal and the movement of the reflection peak thereof;
The functional monomer adopted in the preparation of the inverse opal polymer photonic crystal is a compound containing carboxyl.
2. The method for visually inspecting iron ions using inverse opal polymer photonic crystal according to claim 1, wherein the method for preparing inverse opal polymer photonic crystal comprises the steps of:
Step one, carrying out ultrasonic mixing on SiO 2 particle suspension to obtain SiO 2 dispersion;
Step two, forming a photonic crystal film by a self-assembly method through SiO 2 dispersion liquid;
Step three, mixing a functional monomer, a cross-linking agent and an initiator in a solvent to form a copolymer system, and carrying out ultrasonic treatment to uniformly mix the copolymer system to obtain a precursor solution;
And fourthly, dropwise adding the precursor solution on the photonic crystal film for a plurality of times to uniformly fill the photonic crystal film in the gaps, polymerizing under an ultraviolet lamp, and etching after the polymerization is completed to obtain the inverse opal polymer photonic crystal.
3. The method for visual detection of iron ions using inverse opal polymer photonic crystal according to claim 2, wherein in the first step, siO 2 particles are solid or hollow silica particles having a particle size in the range of 150 to 450 nm;
the solvent used for ultrasonic mixing is ethanol, water or a mixture of the two.
4. The method for visual detection of iron ions by inverse opal polymer photonic crystal according to claim 2, wherein in the second step, the self-assembly method is vertical deposition, spray coating or spin coating.
5. The method for detecting iron ions by using inverse opal polymer photonic crystal visualization according to claim 2, wherein in the third step, the compound containing carboxyl group is acrylic acid, methacrylic acid or itaconic acid.
6. The method for visual detection of iron ions using inverse opal polymer photonic crystal according to claim 2, wherein in step three, the cross-linking agent is ethylene glycol dimethacrylate;
the initiator is a photoinitiator or a thermal initiator;
The solvent is absolute ethanol, glycol or deionized water.
7. The method for visual detection of iron ions by inverse opal polymer photonic crystal according to claim 2, wherein in step three, the molar ratio of the functional monomer to the crosslinking agent in the precursor solution is 5: (0.01-2).
8. The method for visually detecting iron ions by using inverse opal polymer photonic crystal according to claim 2, wherein in the fourth step, the preparation process of the inverse opal polymer photonic crystal specifically comprises the following steps:
Placing the photonic crystal film in a culture dish with an inclined angle, and dripping a precursor solution to the surface of the photonic crystal film a small amount of times to enable the precursor solution to permeate into gaps of the photonic crystal film;
Covering the organic glass sheet soaked by ethanol on a photonic crystal film with a precursor solution on the surface, so that the organic glass sheet, the precursor solution and the photonic crystal film form a sandwich structure, and then placing the organic glass sheet, the precursor solution and the photonic crystal film under an ultraviolet lamp for irradiation to realize photopolymerization and solidification;
And (3) adding a proper amount of hydrofluoric acid solution into a culture dish with a sandwich structure after photopolymerization and solidification, etching silicon dioxide in the photonic crystal film, repeatedly flushing with deionized water after separation, and obtaining the inverse opal polymer photonic crystal after swelling balance and neutrality are achieved.
9. The method for visually inspecting iron ions by using inverse opal polymer photonic crystal according to claim 1, wherein the solution to be inspected is an iron ion solution with a concentration of 1-1000 μm and a ferrous ion solution with a concentration of 10-1000 μm.
10. The method for visually inspecting iron ions by using inverse opal polymer photonic crystal according to claim 1, wherein the concentration of hexamethylenediamine in the mixed system is 9-11mM.
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