CN114672304A - Rice-grade chemiluminescent carbon dot film and preparation method and application thereof - Google Patents
Rice-grade chemiluminescent carbon dot film and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/76—Chemiluminescence; Bioluminescence
Abstract
The invention discloses a preparation method and application of a rice-grade chemiluminescent carbon dot film, belonging to the field of fluorescent carbon nano materials and comprising the following steps: s1, taking citric acid and o-phenylenediamine as raw materials, and carrying out heat treatment at 160-220 ℃ to prepare carbon dots; dissolving polyether F127 in an organic solvent to prepare colloid; s2, mixing the carbon dots prepared in the S1 with the colloid prepared in the S1, adding oxalate peroxide, and stirring uniformly to prepare a chemiluminescent colloid; s3, coating the chemiluminescent colloid prepared in the S2 into a colloid film by a blade coating method or a die method, and evaporating the solvent to obtain the chemiluminescent film. The prepared film can be used in the fields of temperature sensing, information encryption, pattern display and the like, and the application of chemiluminescence is further expanded.
Description
Technical Field
The invention belongs to the technical field of fluorescent carbon nano materials, and particularly relates to a meter-grade chemiluminescent carbon dot film as well as a preparation method and application thereof.
Background
Chemiluminescence, a type of luminescence caused by chemical reactions, has attracted attention from various researchers due to its novel luminescence process. Compared with traditional photoluminescence emission, chemiluminescence emission does not require excitation by high-energy light, thereby avoiding interference of a light excitation process. Therefore, chemiluminescence has been widely used in chemical detection, biological analysis, and cold light sources. However, the application of chemiluminescence is also severely limited by the liquid systems of conventional chemiluminescence reactions. Therefore, the development of novel chemiluminescence state systems and related applications thereof has great value.
The polymer gel can be converted between a solid state and a liquid state due to the special state of the polymer gel, and the gel polymer is used as a substrate material and has extremely high receptivity to various functional structures, so that the polymer gel has wide application in various aspects. For example, in the fields of electronic skin, flexible electronic devices and the like, polymer gels play an important role. The combination of chemiluminescence and polymer gel has greater application value, so that the development of a novel chemiluminescence carbon dot polymer gel film and further demonstration of application of the novel chemiluminescence carbon dot polymer gel film have certain practical significance.
Disclosure of Invention
In order to solve the technical problems, the invention provides a rice-grade chemiluminescent carbon dot film and a preparation method and application thereof.
The invention is realized by the following technical scheme.
The invention provides a preparation method of a rice-scale chemiluminescent carbon dot film, which comprises the following steps:
a preparation method of a rice-scale chemiluminescent carbon dot film comprises the following steps:
s1, using citric acid and o-phenylenediamine as raw materials, and carrying out solvent heat treatment at 160-220 ℃ to prepare carbon dots;
dissolving polyether F127 in an organic solvent to prepare colloid;
s2, mixing the carbon dots prepared in the S1 with the colloid prepared in the S1, adding oxalate peroxide, and stirring uniformly to prepare a chemiluminescent colloid;
s3, coating the chemiluminescent colloid prepared in the S2 into a colloid film by a blade coating method or a die method, and evaporating the solvent to obtain the film.
Preferably, in S1, when preparing the carbon dots, the solvent used is a mixed solvent prepared by mixing water and N, N-dimethylformamide in a volume ratio of 1:1, the mass ratio of citric acid to o-phenylenediamine is 1:1, and the amount ratio of citric acid to mixed solvent is 0.1-1 g: 20 mL.
Preferably, in S1, when preparing the carbon dots, the carbon dots are prepared by performing column chromatography with dichloromethane as a drainage agent after heat preservation at 160-220 ℃ for 10h, collecting the yellow solution precipitated from the first layer, and drying at 40-70 ℃.
Preferably, in S1, the organic solvent used in preparing the colloid is dichloromethane, ethanol, methanol, acetone, ethyl acetate or petroleum ether.
Preferably, in S2, the ratio of carbon dots to colloid is 0.1-0.5g:1L, and the ratio of peroxyoxalate to colloid is 0.5-5g: 1L.
Preferably, in S3, the film size can reach the meter level, and the thickness can be adjusted by the amount of the doctor blade or the glue.
The invention also provides the meter-level chemiluminescent carbon dot film prepared by the preparation method, and after hydrogen peroxide is sprayed on the film, the film generates chemiluminescence, and the chemical strength has temperature response performance.
The meter-level chemiluminescent carbon dot film can be applied to the fields of information encryption, temperature sensing and pattern display.
Compared with the prior art, the invention has the following beneficial effects:
the invention takes citric acid and o-phenylenediamine as raw materials to prepare fluorescent carbon dots, combines a chemiluminescence system with polymer gel for the first time, coats the colloidal film by a blade coating method or a die method to prepare the chemiluminescence carbon dot polymer gel film reaching the meter level, sprays hydrogen peroxide on the film to generate chemiluminescence, and the chemical strength has temperature response performance.
The invention breaks through the liquid system of the traditional chemiluminescence reaction, prepares the chemiluminescence film, has simple preparation method and further expands the application range of chemiluminescence.
Drawings
Fig. 1 is a TEM photograph of the carbon dots prepared in example 1.
Fig. 2 shows a fluorescence spectrum and an absorption spectrum of the carbon dot prepared in example 1.
FIG. 3 is a schematic diagram of the preparation of the film prepared in example 1.
Fig. 4 is a photograph of the film prepared in example 1.
Fig. 5 is an SEM image of the thin film prepared in example 1.
FIG. 6 is a photograph of the meter scale film prepared in example 2.
FIG. 7 is a photograph of the chemiluminescence of the thin film at different temperatures in application example 1.
FIG. 8 shows a chemiluminescence spectrum of the thin film of application example 1.
FIG. 9 is a graph showing the relationship between the emission intensity and the temperature of the thin film in application example 1.
FIG. 10 is a schematic view of thermal imaging of the film in application example 1.
FIG. 11 shows a thermal imaging process of the film of application example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described below with reference to the following specific embodiments and the accompanying drawings, but the embodiments are not meant to limit the present invention.
The experimental methods and the detection methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
The invention provides a preparation method of a rice-scale chemiluminescent carbon dot film, which comprises the following steps:
s1, using citric acid and o-phenylenediamine as raw materials, and carrying out solvent heat treatment at 160-220 ℃ to prepare carbon dots;
dissolving polyether F127 in an organic solvent to prepare colloid;
s2, mixing the carbon dots prepared in the S1 with the colloid prepared in the S1, adding oxalate peroxide, and stirring uniformly to prepare a chemiluminescent colloid;
s3, coating the chemiluminescent colloid prepared in the S2 into a colloid film by a blade coating method or a die method, and evaporating the solvent to obtain the film. The size of the film can reach meter level, the adjustable range of the thickness of the film is 0.1mm-1mm, and the thickness can be adjusted by the amount of a scraper or a colloid.
After the hydrogen peroxide is sprayed on the film, the film generates chemiluminescence, and the chemical strength has temperature response performance.
Example 1
A preparation method of a chemiluminescent carbon dot film comprises the following steps:
(1) at normal temperature, 0.1g of citric acid and 0.1g of o-phenylenediamine (the mass ratio is 1:1) are dissolved in a mixed solution of 10ml of water and 10ml of N, N-dimethylformamide, and a mixed solution is obtained after uniform mixing;
(2) transferring the mixed solution obtained in the step (1) into a polytetrafluoroethylene reaction kettle with the volume of 50ml, then placing the reaction kettle into a forced air drying oven, heating for 10 hours at 200 ℃, naturally cooling to room temperature after the heating, and taking out the solution after reaction;
(3) and (3) performing chromatography on the solution obtained in the step (2) after the reaction by using dichloromethane as a chromatography solution and using 300-mesh silica gel, collecting a yellow solution precipitated from the first layer, drying the solution at 40 ℃, and drying to obtain the carbon dot sample required by people.
Fig. 1 is a TEM photograph of the carbon dots prepared in example 1. As can be seen from FIG. 1, the prepared carbon dots have a particle size of about 2-4nm and a uniform size.
In fig. 2, a and b are fluorescence spectra and absorption spectra of the carbon dots prepared in example 1, respectively. As can be seen from FIG. 2, the carbon dots show stable fluorescence emission and have larger Stokes shift, so that self-absorption can be effectively avoided.
Step 2, preparing a chemiluminescent carbon dot film, as shown in fig. 3, specifically comprising the following steps:
(1) dissolving polyether F127 in dichloromethane, stirring for 2h to completely dissolve the mixture to obtain a colloid, wherein the ratio of the polyether F127 to the dichloromethane is 1g to 50 ml;
(2) mixing the prepared carbon dots with the colloid in the step (1), adding oxalate peroxide, and stirring for 30min to completely and uniformly mix the carbon dots with the colloid to obtain chemiluminescent colloid, wherein the ratio of the carbon dots to the colloid is 0.3g:1L, and the ratio of the oxalate peroxide to the colloid is 1g: 1L;
(3) and (3) coating the chemiluminescent colloid in the step (2) into a colloid film by a blade coating method, and evaporating the solvent at 30-50 ℃ to obtain the chemiluminescent film, wherein the thickness of the film can be adjusted by a scraper, and the thickness in the embodiment is 0.5 mm.
Fig. 4 is a photograph of a film. As can be seen from fig. 4, the film has excellent flexibility and light transmittance, so that the film can be effectively applied to various complex scenes.
In FIG. 5, a and b are SEM images of the thin film at different magnifications, respectively. As can be seen from fig. 5, the film has a porous fiber structure, which can increase the contact area between the film and hydrogen peroxide, thereby improving the chemiluminescence effect of the film.
Example 2
A preparation method of a rice-scale chemiluminescent carbon dot film comprises the following steps:
step 2, preparation of the meter-level chemiluminescent carbon dot film, as shown in fig. 6, the coating steps are as follows:
(1) dissolving polyether F127 in dichloromethane, stirring for 2h to completely dissolve the mixture to obtain a colloid, wherein the ratio of the polyether F127 to the dichloromethane is 1g to 50 ml;
(2) mixing the prepared carbon dots with colloid, adding oxalate peroxide, and stirring for 30min to obtain chemiluminescent colloid, wherein the ratio of carbon dots to colloid is 0.3g:1L, and the ratio of oxalate peroxide to colloid is 1g: 1L;
(3) pouring the chemiluminescent colloid in the step (2) into a meter-level plastic mold, uniformly paving the colloid film into a colloid film, and evaporating the solvent at room temperature to obtain the chemiluminescent film, wherein the thickness of the film can be adjusted by the amount of the chemiluminescent colloid poured, the size of the film can be determined by the size of the mold in the method for preparing the chemiluminescent film by adopting a mold method, and the meter-level film can be prepared under laboratory conditions; the diagonal length of the film produced in this example was 1.18 m and the thickness was 0.5 mm.
Example 3
A preparation method of a rice-scale chemiluminescent carbon dot film comprises the following steps:
(1) at normal temperature, 1g of citric acid and 1g of o-phenylenediamine (the mass ratio is 1:1) are dissolved in a mixed solution of 10ml of water and 10ml of N, N-dimethylformamide, and a mixed solution is obtained after uniform mixing;
(2) transferring the mixed solution obtained in the step (1) to a polytetrafluoroethylene reaction kettle with the volume of 50ml, then placing the reaction kettle in an air-blowing drying oven, heating for 10 hours at 160 ℃, naturally cooling to room temperature after the heating, and taking out the reacted solution;
(3) performing chromatography on the reacted solution obtained in the step (2) by using 300-mesh silica gel by using dichloromethane as a chromatographic solution, collecting a yellow solution precipitated from the first layer, drying the solution at 70 ℃, and obtaining a carbon dot sample required by people after drying;
step 2, preparing the meter-level chemiluminescence carbon dot film, comprising the following steps:
(1) dissolving polyether F127 in dichloromethane, stirring for 2h to completely dissolve the mixture to obtain a colloid, wherein the ratio of the polyether F127 to the dichloromethane is 1g:50 ml;
(2) mixing the prepared carbon dots with colloid, adding oxalate peroxide, and stirring for 30min to obtain chemiluminescent colloid, wherein the ratio of carbon dots to colloid is 0.1g:1L, and the ratio of oxalate peroxide to colloid is 0.5g: 1L;
(3) and (3) pouring the chemiluminescent colloid in the step (2) into a meter-level plastic mold, uniformly paving the colloid film, evaporating the solvent at room temperature to obtain the chemiluminescent film, wherein the thickness of the film can be adjusted by the amount of the chemiluminescent colloid poured, the size of the film can be determined by the size of the mold in the method for preparing the chemiluminescent film by adopting a mold method, and the meter-level film can be prepared under laboratory conditions.
Example 4
A preparation method of a rice-scale chemiluminescent carbon dot film comprises the following steps:
(1) at normal temperature, 0.5g of citric acid and 0.5g of o-phenylenediamine (the mass ratio is 1:1) are dissolved in a mixed solution of 10ml of water and 10ml of N, N-dimethylformamide, and a mixed solution is obtained after uniform mixing;
(2) transferring the mixed solution obtained in the step (1) into a polytetrafluoroethylene reaction kettle with the volume of 50ml, then placing the reaction kettle into a forced air drying oven, heating for 10 hours at 220 ℃, naturally cooling to room temperature after the heating, and taking out the solution after reaction;
(3) performing chromatography on the reacted solution obtained in the step (2) by using 300-mesh silica gel by using dichloromethane as a chromatographic solution, collecting a yellow solution precipitated from the first layer, drying the solution at 70 ℃, and obtaining a carbon dot sample required by people after drying;
step 2, preparing the meter-level chemiluminescent carbon dot film, which comprises the following steps:
(1) dissolving polyether F127 in dichloromethane, stirring for 2h to completely dissolve the mixture to obtain a colloid, wherein the ratio of the polyether F127 to the dichloromethane is 1g to 50 ml;
(2) mixing the prepared Carbon Dots (CD) with colloid, adding oxalate peroxide (CPPO), stirring for 30min to completely mix uniformly to obtain chemiluminescent colloid, wherein the ratio of the carbon dots to the colloid is 0.5g:1L, and the ratio of the oxalate peroxide to the colloid is 5g: 1L;
(3) and (3) pouring the chemiluminescent colloid in the step (2) into a meter-level plastic mold, uniformly paving the meter-level plastic mold into a colloid film, and evaporating the solvent at room temperature to obtain the chemiluminescent film, wherein the thickness of the film can be adjusted by the amount of the chemiluminescent colloid poured, the size of the film can be determined by the size of the mold in the method for preparing the chemiluminescent film by adopting a mold method, and the meter-level film is prepared under laboratory conditions.
Application example 1
Temperature imaging application of chemiluminescence carbon dot film
step 2, the chemiluminescent film of the embodiment 2 is coated on the surface of an object, hydrogen peroxide solution is sprayed on the surface of the film, the film generates chemiluminescence, and the chemical intensity of the film presents a bright and dark image along with the temperature distribution of the object.
And 3, taking a chemiluminescence photo by using a mobile phone, and processing the photo by using a preset program to obtain a temperature distribution image of the object.
FIG. 7 is a photograph of the chemiluminescence of the film at different temperatures. As can be seen from fig. 7, the films showed significant chemiluminescent intensities at different temperatures, indicating that the prepared films exhibited excellent temperature response properties.
FIG. 8 is a chemiluminescence spectrum of a thin film. As can be seen from FIG. 8, after the carbon dots are doped, the film shows a distinct chemiluminescence peak of the carbon dots, indicating that the chemiluminescence of the film comes from the carbon dots.
FIG. 9 is a graph of the luminescence intensity of a thin film as a function of temperature. As can be seen from FIG. 9, the chemiluminescence of the thin film has a good response relationship with temperature, and a significant linear relationship is shown between 15 and 55 degrees Celsius, so that the thin film can be used for temperature sensing and imaging.
FIG. 10 is a schematic thermal image of a film. As can be seen from fig. 10, the film can be effectively applied to temperature imaging, and in the palm example, chemiluminescence temperature imaging of the palm has been successfully achieved. This demonstrates that chemiluminescent films are feasible for temperature imaging.
FIG. 11 is a thermal imaging process for thin films. As can be seen from fig. 11, a relation between the chemiluminescence intensity and the temperature is constructed and then introduced into the mobile phone APP, so that a simple temperature measurement imaging system using the mobile phone as a temperature measurement processing platform is realized.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, it is intended that such changes and modifications be included within the scope of the appended claims and their equivalents.
Claims (10)
1. A preparation method of a rice-scale chemiluminescent carbon dot film is characterized by comprising the following steps:
s1, taking citric acid and o-phenylenediamine as raw materials, and carrying out solvent heat treatment at 160-220 ℃ to prepare carbon dots;
dissolving polyether F127 in an organic solvent to prepare colloid;
s2, mixing the carbon dots prepared in the S1 with the colloid prepared in the S1, adding oxalate peroxide, and stirring uniformly to prepare a chemiluminescent colloid;
and S3, coating the chemiluminescent colloid prepared in the S2 into a colloid film by a blade coating method or a die method, and evaporating the solvent to obtain the meter-level chemiluminescent carbon dot film.
2. The method for producing a meter-level chemiluminescent carbon dot film according to claim 1, wherein in S1, the solvent used in the carbon dot production is a mixed solvent prepared by mixing water and N, N-dimethylformamide in a volume ratio of 1:1, the mass ratio of citric acid to o-phenylenediamine is 1:1, and the amount ratio of citric acid to mixed solvent is 0.1-1 g: 20 mL.
3. The method for preparing the meter-level chemiluminescent carbon dot film as defined in claim 1, wherein in S1, the carbon dot is prepared by performing column chromatography with dichloromethane as a drainage agent after heat preservation at 160-220 ℃ for 10h, collecting the yellow solution precipitated from the first layer, and drying at 40-70 ℃ to obtain the carbon dot.
4. The method of claim 1, wherein the organic solvent used in the preparation of the colloid in S1 is dichloromethane, ethanol, methanol, acetone, ethyl acetate, or petroleum ether.
5. The method for preparing a meter-level chemiluminescent carbon dot film according to claim 1, wherein in S2, the ratio of carbon dots to colloid is 0.1-0.5g:1L, and the ratio of oxalate peroxide to colloid is 0.5-5g: 1L.
6. The method of claim 1, wherein the size of the prepared film is in the order of meter, and the thickness of the prepared film is adjusted by the amount of the doctor blade or the colloid in the step S3.
7. The meter-sized chemiluminescent carbon dot film produced by the process according to any one of claims 1 to 6 wherein the film produces chemiluminescence and the chemical strength has temperature response properties after hydrogen peroxide is sprayed on the produced film.
8. Use of the meter-sized chemiluminescent carbon dot film of claim 7 in the field of information encryption.
9. Use of the meter-sized chemiluminescent carbon dot film of claim 7 in the field of temperature sensing.
10. Use of the meter-sized chemiluminescent carbon dot film of claim 7 in the field of graphic displays.
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