CN112745838A - Large-scale solid green fluorescent carbon nanodots and preparation method thereof - Google Patents
Large-scale solid green fluorescent carbon nanodots and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of large-scale solid green fluorescent carbon nanodots, and belongs to the technical field of fluorescent carbon nanodot materials. The method comprises the following steps: uniformly dispersing a carbon source and a dispersing agent in a water solvent, adding an inorganic crystal, uniformly mixing, and carrying out microwave reaction at 100-200 ℃ for 3-30 min to obtain the carbon nanodots; the inorganic crystal is potassium hydroxide or potassium citrate. According to the invention, by introducing inorganic crystals such as potassium hydroxide or potassium citrate, the problem of fluorescence quenching of the carbon dots in a solid state is successfully inhibited, the in-situ limited-growth of the solid luminescent carbon nanodots is realized, the carbon dots are green fluorescence in the solid state, and the fluorescence efficiency can reach 75.9% at most.
Description
Technical Field
The invention belongs to the technical field of fluorescent carbon nano-dot materials, and particularly relates to a large-scale solid green fluorescent carbon nano-dot and a preparation method thereof.
Background
Fluorescent powder, a class of substances that can emit fluorescence under illumination, is visible everywhere in our lives, and particularly in the field of lighting, fluorescent powder plays an extremely important role. At present, the fluorescent powder used for lighting is mainly rare earth fluorescent powder, however, the rare earth fluorescent powder also faces the outstanding problems of high price, environmental pollution, high recycling cost, difficult adjustment of light-emitting wavelength and the like, and along with the gradual improvement of the demand of people for lighting, people are urgently required to develop a green low-cost substitute of the rare earth fluorescent powder.
As a novel nano fluorescent material, the fluorescent carbon nanodots (carbon dots) have the outstanding advantages of high luminous efficiency, easy adjustment of luminous wavelength, simple preparation method, low cost, low toxicity, degradability, no pollution and the like, and the preparation of the green environment-friendly light source based on the carbon dot fluorescent powder is possible. At present, there are many researches on carbon dots, and in the development of the carbon dots, a key problem is fluorescence quenching of the carbon dots in a solid state, which also directly restricts the application of the carbon dots in the field of solid state lighting. Therefore, how to realize the rapid and large-scale preparation of the solid-state carbon dot fluorescent powder with high luminous efficiency is the central importance for the development of carbon dot-based green environmental protection illumination.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a large-scale solid green fluorescent carbon nanodot, which solves the problems that the rapid large-scale preparation is difficult to realize due to fluorescence quenching in a solid state of a carbon dot.
The invention aims to provide a preparation method of large-scale solid green fluorescent carbon nanodots, which comprises the following steps: uniformly dispersing a carbon source and a dispersing agent in a water solvent, adding an inorganic crystal, uniformly mixing, and carrying out microwave reaction at 100-200 ℃ for 3-30 min to obtain the carbon nanodots;
the inorganic crystal is sodium hydroxide, sodium citrate, potassium hydroxide or potassium citrate.
Preferably, the microwave reaction power is 700-800W, the heating rate is 7.5-17.5K/s, and the microwave wavelength is 2.45 GHz.
Preferably, the mass ratio of the carbon source to the dispersing agent is 1: 1.5-2.5.
More preferably, the carbon source is citric acid.
More preferably, the dispersant is urea.
Preferably, the mass ratio of the inorganic crystal to the carbon source is 1: 0.4-0.8.
Preferably, a microwave oven or a microwave reactor is adopted in the microwave reaction process.
The second purpose of the invention is to provide a large-scale solid green fluorescent carbon nanodot.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method provided by the invention, by introducing inorganic crystals such as potassium hydroxide or potassium citrate, the problem of fluorescence quenching of the carbon dots per se in a solid state is successfully inhibited, the in-situ limited growth of the solid luminescent carbon nanodots is realized, the carbon dots are green fluorescence in the solid state, and the fluorescence efficiency can reach 75.9% at most;
the preparation method provided by the invention can realize rapid large-scale preparation of the fluorescent carbon dots, in the method, the preparation of 13g of samples can be realized at one time, the preparation time only needs about 10min, and the yield of the carbon dot powder can be doubled by further increasing the reaction container;
the green carbon dots prepared by the preparation method provided by the invention have high yield of 70%;
the carbon dots prepared by the preparation method provided by the invention have strong illumination stability, and the luminous intensity is only reduced by 3.3% after continuous illumination for 72 hours.
Drawings
Fig. 1 is a schematic flow chart of a large-scale solid-state green fluorescent carbon nanodot preparation method provided by the embodiment.
FIG. 2 is a photograph of the carbon nanodots obtained in examples 1 to 3 under sunlight and irradiation of an ultraviolet lamp;
wherein, the picture A and the picture A1 are the photos of the carbon nanodots obtained in the example 1 under an ultraviolet lamp and sunlight respectively; fig. B and B1 are photographs of the carbon nanodots obtained in example 2 under an ultraviolet lamp and sunlight, respectively; fig. C and C1 are photographs of the carbon nanodots obtained in example 3 under an ultraviolet lamp and sunlight, respectively.
FIG. 3 is an optical photograph of the carbon nanodots obtained in example 4; wherein, the picture A and the picture B are the pictures of the carbon nanodots obtained in the example 4 under the sunlight; fig. C is a photograph of the carbon nanodots obtained in example 4 under an ultraviolet lamp.
Fig. 4 is a TEM image of the carbon nanodots obtained in example 4.
Fig. 5 is a high-resolution TEM image of the carbon nanodots obtained in example 4.
Fig. 6 is a light emission spectrum under ultraviolet excitation of the carbon nanodots obtained in example 4.
Fig. 7 is a graph of intensity comparison of light emission spectra of the carbon nanodots obtained in example 4 after continuously receiving the uv light for 72 hours and 0 hour.
Fig. 8 is a mechanism diagram of improvement of solid-state light emitting performance after inorganic crystals are introduced into the carbon nanodots provided in example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood and enable those skilled in the art to practice the present invention, the following embodiments are further described, but the present invention is not limited to the following embodiments.
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.
Example 1
A preparation method of a large-scale solid green fluorescent carbon nanodot is shown in figure 1 and comprises the following steps:
step A, dissolving 1g of citric acid and 2g of urea in 20ml of deionized water, and carrying out ultrasonic treatment on the mixed solution at normal temperature for about 3min to obtain a transparent colorless solution;
step B, adding 0.4g of sodium hydroxide into the solution obtained in the step A, and fully stirring until all reactants are dissolved;
and step C, placing the solution obtained in the step B in a common microwave oven, heating the solution in the beaker by microwaves at 750w for reaction for 3min, finishing the reaction when the solution in the beaker is evaporated to dryness and a green foamy solid is generated, and naturally cooling the reactant at normal temperature, wherein the green foamy solid is the prepared fluorescent carbon nanodot.
The specific operating procedure of this example is shown in FIG. 1, where a total of 2.2g of carbon points are obtained.
Example 2
A preparation method of large-scale solid green fluorescent carbon nanodots comprises the following steps:
step A, dissolving 1g of citric acid and 2g of urea in 20ml of deionized water, and carrying out ultrasonic treatment on the mixed solution at normal temperature for about 3min to obtain a transparent colorless solution;
step B, adding 0.6g of potassium hydroxide into the solution obtained in the step A, and fully stirring until all reactants are dissolved;
and step C, placing the solution obtained in the step B in a common microwave oven, heating the solution in the beaker by microwaves at 800w for reaction for 3min, finishing the reaction when the solution in the beaker is evaporated to dryness and a green foamy solid is generated, and naturally cooling the reactant at normal temperature, wherein the green foamy solid is the prepared fluorescent carbon nanodot.
The specific operating procedure of this example is shown in FIG. 1, where a total of 2.4g of carbon points are obtained.
Example 3
A preparation method of large-scale solid green fluorescent carbon nanodots comprises the following steps:
step A, dissolving 1g of citric acid and 2g of urea in 20ml of deionized water, and carrying out ultrasonic treatment on the mixed solution at normal temperature for about 3min to obtain a transparent colorless solution;
step B, adding 0.8g of sodium hydroxide into the solution obtained in the step A, and fully stirring until all reactants are dissolved;
and step C, placing the solution obtained in the step B in a common microwave oven, heating the solution in the microwave oven at 700w for reaction for 3min, finishing the reaction when the solution in the beaker is evaporated to dryness and a green foamy solid is generated, and naturally cooling the reactant at normal temperature, wherein the green foamy solid is the prepared fluorescent carbon nanodot.
The specific operating procedure of this example is shown in FIG. 1, where a total of 2.7g of carbon points are obtained.
Example 4
A preparation method of large-scale solid green fluorescent carbon nanodots comprises the following steps:
step A, dissolving 5g of citric acid and 10g of urea in 100ml of deionized water, and carrying out ultrasonic treatment on the mixed solution at normal temperature for about 3min to obtain a transparent colorless solution;
step B, adding 4g of potassium hydroxide into the solution obtained in the step A, and fully stirring until the reactants are completely dissolved;
and step C, placing the solution obtained in the step B in a common microwave oven, heating the solution in the microwave oven at 700w for reaction for 10min, finishing the reaction when the solution in the beaker is evaporated to dryness and a green foamy solid is generated, and naturally cooling the reactant at normal temperature, wherein the green foamy solid is the prepared fluorescent carbon nanodot.
The specific operating procedure of this example is shown in FIG. 1, which gives a total of 13g carbon points.
Example 5
A preparation method of large-scale solid green fluorescent carbon nanodots comprises the following steps:
step A, dissolving 100g of citric acid and 200g of urea in 2L of deionized water, and carrying out ultrasonic treatment on the mixed solution at normal temperature for about 5min to obtain a transparent colorless solution;
step B, adding 80g of potassium citrate into the solution obtained in the step A, and fully stirring until the reactants are completely dissolved;
and step C, placing the solution obtained in the step B in a common microwave oven, heating the solution in the beaker by the microwave for reaction for about 30min at 750w, finishing the reaction when the solution in the beaker is evaporated to dryness and a green foamy solid is generated, and naturally cooling the reactant at normal temperature, wherein the green foamy solid is the prepared fluorescent carbon nanodot.
Example 6
A preparation method of large-scale solid green fluorescent carbon nanodots comprises the following steps:
step A, dissolving 5g of citric acid and 10g of urea in 100ml of deionized water, and carrying out ultrasonic treatment on the mixed solution at normal temperature for about 3min to obtain a transparent colorless solution;
step B, adding 4g of sodium citrate into the solution obtained in the step A, and fully stirring until the reactants are completely dissolved;
and step C, placing the solution obtained in the step B in a common microwave oven, heating the solution in the beaker by the microwave for reaction for about 10min at 750w, finishing the reaction when the solution in the beaker is evaporated to dryness and a green foamy solid is generated, and naturally cooling the reactant at normal temperature, wherein the green foamy solid is the prepared fluorescent carbon nanodot.
In order to illustrate the relevant performance of the large-scale solid-state green fluorescent carbon nanodots prepared by the preparation method provided by the invention, the large-scale solid-state green fluorescent carbon nanodots provided in the embodiments 1 to 4 are tested, and the reason for introducing the solid-state luminescent performance improvement of the inorganic crystal is analyzed, as shown in fig. 2 to 8;
FIG. 2 is a photograph of the sample obtained in examples 1 to 3 under sunlight and irradiation of an ultraviolet lamp;
wherein, FIG. A and FIG. A1 are photographs of the sample obtained in example 1 under ultraviolet lamp and sunlight, respectively;
FIGS. B and B1 are photographs of the sample obtained in example 2 under UV light and sunlight, respectively;
fig. C and C1 are photographs of the sample obtained in example 3 under uv light and sunlight, respectively.
As can be seen from FIG. 2, in the sunlight, the examples 1 to 3 are all yellow-green powders, and under the irradiation of ultraviolet light, the three samples can emit bright green fluorescence, and under the irradiation of ultraviolet light with the same intensity, the fluorescence intensity of the three samples is sequentially enhanced.
FIG. 3 is an optical photograph of a sample obtained in example 4. Wherein, the pictures A and B are the pictures under the natural light, the picture C is the picture under the ultraviolet irradiation, as can be seen from figure 3, under the natural light, the prepared carbon nanodots present yellow green, can emit bright green fluorescence under the ultraviolet irradiation.
Fig. 4 and 5 are a TEM image and a high-resolution TEM image of the sample obtained in example 4, respectively, and it can be seen from fig. 4 and 5 that the carbon dots are a point-like structure with good dispersibility in a microscopic scale, and the crystal grain size thereof is about 5 nm.
FIG. 6 is a luminescence spectrum of a sample obtained in example 4 under ultraviolet excitation, which has an emission wavelength of 510nm corresponding to a green wavelength band.
FIG. 7 is a graph showing intensity comparison of luminescence spectra of the sample obtained in example 4 after continuously receiving UV light for 72 hours and 0 hour. As can be seen from the graph, the luminescence wavelength of the sample is still at 510nm after continuous UV irradiation for 72 hours, and the luminescence intensity is reduced by only 3.3%.
Fig. 8 is a mechanism diagram of improvement of solid-state light emitting performance after inorganic crystals are introduced into the carbon nanodots provided in example 1. As can be seen from fig. 8, after the inorganic crystal is introduced, the carbon dots are independently dispersed and confined in the inorganic crystal space, the coupling interaction between the carbon dots is weakened, the energy transfer effect is reduced, and the solid-state light emission intensity is remarkably enhanced.
In conclusion, the preparation method provided by the invention successfully inhibits the problem of fluorescence quenching of the carbon dots in a solid state by introducing inorganic crystals such as potassium hydroxide or potassium citrate, realizes green fluorescence of the carbon dots in the solid state, and has the highest fluorescence efficiency of 75.9%;
the preparation method provided by the invention can realize rapid large-scale preparation of the fluorescent carbon dots, in the method, the preparation of 13g of samples can be realized at one time, the preparation time only needs about 10min, and the yield of the carbon dot powder can be doubled by further increasing the reaction container;
the green carbon dots prepared by the preparation method provided by the invention have high yield of 70%;
the carbon dots prepared by the preparation method provided by the invention have strong illumination stability, and the luminous intensity is only reduced by 3.3% after continuous illumination for 72 hours.
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 (8)
1. A preparation method of large-scale solid green fluorescent carbon nanodots is characterized by comprising the following steps:
uniformly dispersing a carbon source and a dispersing agent in a water solvent, adding an inorganic crystal, uniformly mixing, and carrying out microwave reaction at 100-200 ℃ for 3-30 min to obtain the carbon nanodots;
the inorganic crystal is sodium hydroxide, sodium citrate, potassium hydroxide or potassium citrate.
2. The method for preparing the scale solid-state green fluorescent carbon nanodots according to claim 1, wherein the microwave reaction power is 700-800W, the heating rate is 7.5-17.5K/s, and the microwave wavelength is 2.45 GHz.
3. The method for preparing the scale solid-state green fluorescent carbon nanodots according to claim 1, wherein the mass ratio of the carbon source to the dispersing agent is 1: 1.5-2.5.
4. The method for preparing scale solid-state green fluorescent carbon nanodots according to claim 3, wherein the carbon source is citric acid.
5. The method for preparing scaled solid-state green fluorescent carbon nanodots according to claim 3, wherein the dispersant is urea.
6. The method for preparing the scale solid-state green fluorescent carbon nanodots according to claim 1, wherein the mass ratio of the inorganic crystal to the carbon source is 1: 0.4-0.8.
7. The method for preparing scaled solid-state green fluorescent carbon nanodots according to claim 1, wherein a microwave oven or a microwave reactor is used in the microwave reaction process.
8. A large-scale solid green fluorescent carbon nanodot prepared by the preparation method of any one of claims 1 to 7.
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| CN114214063A (en) * | 2021-12-17 | 2022-03-22 | 华东师范大学 | Preparation method of single-matrix white light emitting carbon dot fluorescent powder |
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