CN112391163A - Nitrogen-doped yellow carbon quantum dot and preparation method thereof - Google Patents
Nitrogen-doped yellow carbon quantum dot and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nitrogen-doped yellow carbon quantum dot and a preparation method thereof, wherein the particle size range of a yellow carbon quantum dot fluorescent material is 3-6 nm. The yellow carbon quantum can emit bright yellow fluorescence under the excitation of light with the wavelength of 320-550 nm, and the fluorescence quantum efficiency can reach 38 percent at most. The preparation method takes 2,4, 6-trihydroxybenzoic acid as a carbon source, m-phenylenediamine as a nitrogen source and tin salt as a catalyst, so that the synthesis time for synthesizing the yellow carbon quantum dots is greatly shortened, and the absolute fluorescence quantum efficiency of the synthesized yellow carbon quantum dots is high. The yellow carbon quantum dots prepared by the method have stable fluorescence performance in an ethanol solution, and no fluorescence intensity reduction is observed within 35 days. The preparation method greatly simplifies the synthesis process of synthesizing the yellow carbon quantum dots, improves the preparation efficiency and greatly reduces the preparation cost.
Description
Technical Field
The invention relates to a carbon quantum dot and a preparation method thereof, in particular to a yellow carbon quantum dot and a preparation method thereof, which are applied to the technical field of carbon nano materials.
Background
The carbon quantum dots are spherical-like nano materials with the particle size of less than 10 nm. The carbon quantum dots not only have the luminescent property and small-size characteristic of the traditional quantum dots, but also have the advantages of good water solubility, stable luminescent property, good compatibility with biomolecules, small-molecule chemical reagents, generated material materials and the like in synthetic raw materials, simple synthetic method, low cost and the like. The characteristics lead the fluorescent probe to have wide application prospect in the fields of biological imaging, luminescent marking of biomedical molecules, fluorescent sensors and the like.
There are many methods for synthesizing carbon quantum dots, and the chemical synthesis methods include hydrothermal method, solvothermal method, microwave method, and the like. Wherein, the carbon quantum dot luminescent material synthesized by the solvothermal method has the advantages of narrow particle size distribution and high fluorescence quantum efficiency. However, the reaction time for synthesizing carbon quantum dots by the solvothermal method reported at present needs a long time, and the quantum efficiency is mostly not high. The literature reports that the quantum efficiency of the yellow-green carbon quantum dots (the maximum emission wavelength is 555nm and the maximum excitation wavelength is 393nm) which can be synthesized by a microwave method by using resorcinol as a carbon source and using o-phenylenediamine as a nitrogen source is 62.2% (PeiYang, ZiqiZhu, Xinghui Li, et. J. alloys Compd.2020,834: 154399.). The carbon quantum dots with yellow green color (the maximum emission wavelength is 555nm and the maximum excitation wavelength is 450nm) are thermally synthesized by using citric acid as a carbon source, urea as a nitrogen source, manganese acetate as a catalyst and toluene as a solvent, and the quantum luminous efficiency reaches 68.6 percent (Yingbo Liu, Daiyong Chao, Liang Zhou, et al. Carbon,2018,135: 253-259). Therefore, the novel preparation method of the carbon quantum dot luminescent material which is green and environment-friendly, short in synthesis time, low in cost, uniform in particle size distribution and high in quantum efficiency is found, and the method has important research significance and practical value for wide and practical application of the carbon quantum dot. The penetration of short wavelength emitted fluorescence and damage to biological tissues limit its application in the biological field. Therefore, the synthesis of carbon quantum dots excited by longer wavelength and emitted by longer wavelength has important significance, and becomes a technical problem to be solved urgently.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects of the prior art and provide the nitrogen-doped yellow carbon quantum dot and the preparation method thereof. The preparation method can synthesize the high-quality nitrogen-doped yellow carbon quantum dot material with longer excitation wavelength and uniform granularity, greatly simplifies the synthesis process of synthesizing the yellow carbon quantum dot, improves the preparation efficiency and greatly reduces the preparation cost.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
the nitrogen-doped yellow carbon quantum dot has the particle size range of 3-6 nm, and can emit yellow fluorescence under the excitation of light with the particle size range of 320-550 nm; the nitrogen-doped yellow carbon quantum dots are dispersed in an ethanol solution, and the fluorescence intensity is not reduced within 35 days.
Preferably, the maximum excitation wavelength at which the nitrogen-doped yellow carbon quantum dots of the present invention emit yellow fluorescence is 525 nm.
Preferably, the nitrogen-doped yellow carbon quantum dot can emit yellow fluorescence under the excitation of light with the wavelength of 336-525 nm.
Preferably, the nitrogen-doped yellow carbon quantum dots emit yellow fluorescence at a maximum emission wavelength of 568 nm.
Preferably, the surface of the nitrogen-doped yellow carbon quantum dot is combined with-COOH, -OH and-NH2A group.
The invention relates to a preparation method of nitrogen-doped yellow carbon quantum dots, which synthesizes the yellow carbon quantum dots by using 2,4, 6-trihydroxybenzoic acid as a carbon source, m-phenylenediamine as a nitrogen source and metallic tin salt as a catalyst and adopting a solvothermal method, and comprises the following steps:
a. according to the molar ratio of the metallic tin salt to the 2,4, 6-trihydroxybenzoic acid of 1: (1-2), dissolving a metal tin salt and 2,4, 6-trihydroxybenzoic acid in ethanol, and adding a certain amount of m-phenylenediamine to form a mixed solution; the mol ratio of the m-phenylenediamine to the 2,4, 6-trihydroxybenzoic acid is 1: (1-2); adjusting the pH value of the mixed solution to 4-6, and stirring for 30-60 minutes at 40-70 ℃ to uniformly mix the solution;
b. putting the uniformly mixed solution into a polytetrafluoroethylene reaction kettle, reacting for 2-4 hours at 160-200 ℃, and then cooling to room temperature to obtain a product solution;
c. and (3) carrying out centrifugal separation treatment on the product solution, removing tin oxide, dialyzing by using a membrane with the molecular weight of 3500Da for at least 1 day, and removing small molecular substances, thereby obtaining the nitrogen-doped yellow carbon quantum dots.
Preferably, yellow carbon quantum dots with high fluorescence quantum efficiency can be synthesized, and the maximum absolute fluorescence quantum efficiency reaches 38%.
Preferably, in the step a, the tin salt adopts SnCl4·5H2O、SnCl4、SnCl2·2H2O、SnCl2And SnF2Any one salt or a mixed salt of any two thereof.
Preferably, in the step a, 1-2 mmol of 2,4, 6-trihydroxybenzoic acid and tin salt are dissolved in at least 20mL of ethanol.
Preferably, in the step b, the reaction is carried out at 160-180 ℃.
Preferably, in the step c, the concentration of the obtained nitrogen-doped yellow carbon quantum dot solution is not lower than 23 mg/mL.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the method takes 2,4, 6-trihydroxybenzoic acid as a carbon source, m-phenylenediamine as a nitrogen source and a metallic tin compound as a catalyst, and mixes nitrogen atoms in a carbon quantum dot to ensure that the light-emitting wavelength is red-shifted to a yellow light-emitting region and improve the light-emitting efficiency of the carbon quantum dot; the invention takes the metallic tin compound as the catalyst, greatly shortens the synthesis time of the carbon quantum dots and greatly reduces the synthesis cost of the carbon quantum dots; the synthesis time is shortened by more than 50% compared with the time reported by a literature, and the quantum efficiency of the yellow carbon quantum dot synthesized in 2 hours can reach 38%;
2. the synthesis method is carried out in the air, complex synthesis equipment is not needed, and chromatographic separation is not needed; the synthesis method has the advantages of high synthesis efficiency and low cost; the method does not use a sulfur-containing chemical reagent, and is a green and environment-friendly synthesis method;
3. the yellow carbon quantum dot fluorescent material synthesized by the method has stable fluorescence performance in an ethanol solution, and the phenomenon of fluorescence intensity reduction is not observed within 35 days; the luminous performance is not weakened in the air, bright yellow fluorescence is emitted under the excitation of light with the wavelength of 320-550 nm, and the maximum emission wavelength is 568 nm; the stability of the luminescent property of the yellow carbon quantum dot under the room temperature condition is good; the method is simple and easy to implement, low in cost and suitable for popularization and application.
Drawings
FIG. 1 is a fluorescence emission spectrum of a yellow fluorescent carbon quantum dot obtained in an embodiment of the present invention under 336nm, 380nm and 525nm light excitation, respectively, and the inset is a photograph of the yellow fluorescent carbon quantum dot emitting yellow fluorescence under 365nm lamp illumination.
FIG. 2 shows an excitation spectrum of a yellow fluorescent carbon quantum dot obtained in an embodiment of the present invention at a detection wavelength of 568 nm.
Fig. 3 is an ultraviolet-visible absorption spectrum of the yellow fluorescent carbon quantum dot ethanol solution obtained in the first embodiment of the present invention, and the inset is a photograph of the yellow fluorescent carbon quantum dot ethanol solution under natural light.
Fig. 4 is a high-resolution tem image of the yellow fluorescent carbon quantum dot obtained in the first embodiment of the present invention, and the inset shows the characteristic lattice diffraction fringes of the carbon quantum dot.
Fig. 5 is a particle size distribution diagram of the yellow fluorescent carbon quantum dots obtained in the first embodiment of the present invention.
Fig. 6 is an infrared spectrum of the yellow fluorescent carbon quantum dot obtained in the first embodiment of the present invention.
FIG. 7 is a time-dependent fluorescence intensity curve of yellow fluorescent carbon quantum dots at 568nm emission wavelength according to an embodiment of the present invention.
Fig. 8 is a schematic flow chart of a method for preparing nitrogen-doped yellow carbon quantum dots according to an embodiment of the present invention, and the inset shows a photograph of the yellow fluorescent light emitted under 365nm lamp illumination.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
the first embodiment is as follows:
in this example, referring to fig. 7, a method for preparing nitrogen-doped yellow carbon quantum dots, which uses 2,4, 6-trihydroxybenzoic acid as a carbon source, m-phenylenediamine as a nitrogen source, and a metallic tin salt as a catalyst, and synthesizes yellow carbon quantum dots by a solvothermal method, includes the following steps:
a. weighing 1mmol of SnCl4·5H2Dissolving O and 1mmol of 2,4, 6-trihydroxybenzoic acid in 15mL of absolute ethanol, and heating to 40 ℃ under magnetic stirring to obtain a carbon source reactant solution; dissolving 2mmol of m-phenylenediamine in 5mL of absolute ethanol to form a nitrogen source reactant solution; dropwise adding the carbon source reactant solution into a nitrogen source reactant solution, and adjusting the pH value of the solution to 6; stirring at 40 deg.C for 60 min to mix the solution uniformly;
b. putting the uniformly mixed solution into a polytetrafluoroethylene reaction kettle, reacting for 2 hours at 180 ℃, and naturally cooling to room temperature to obtain a product solution;
c. and (3) performing centrifugal separation treatment on the product solution at the speed of 10000 r/min to remove tin oxide nanoparticles generated by the reaction, dialyzing for 1 day by using a membrane with the molecular weight of 3500Da, and removing small molecular substances, thereby obtaining the nitrogen-doped yellow carbon quantum dot solution with the nitrogen-doped yellow carbon quantum dot concentration of 23 mg/mL.
Experimental test analysis:
the nitrogen-doped yellow carbon quantum dot solution prepared in the example is used as a test sample for analysis test and property inspection,
after the yellow carbon quantum dots prepared in this example were diluted 100 times with ethanol, their fluorescence emission spectra under excitation of 336nm, 380nm, and 525nm light, respectively, were measured with a steady-state transient fluorescence spectrometer FLS1000, see fig. 1. The maximum emission of the yellow carbon quantum dot is 568nm, the maximum emission wavelength is not changed along with the excitation wavelength, and the yellow carbon quantum dot emits characteristic yellow fluorescence.
Under the detection wavelength of 568nm, the dilute ethanol solution of the yellow carbon quantum dots has three excitation absorption peaks of 336nm, 380nm and 525nm, and as shown in figure 2, the yellow carbon quantum dots can obtain bright yellow fluorescence under the excitation of light of 320 nm-550 nm.
FIG. 3 is the UV-VIS absorption spectrum of the yellow carbon quantum dot prepared in this example, which shows that it has three main absorption peaks at 273nm, 293nm and 425 nm. Fig. 4 is a high resolution electron microscopy HRTEM of the yellow carbon quantum dot prepared in this example, with characteristic lattice diffraction fringes of the carbon quantum dot. FIG. 5 is a particle size distribution diagram of the yellow fluorescent carbon quantum dots obtained in this example, which shows that the particle size of the carbon quantum dots ranges from 3nm to 6 nm. FIG. 6 is an infrared absorption spectrum of the yellow carbon quantum dot obtained in the present example, which shows that the carbon quantum dot has a large amount of-COOH and-OH groups on the surface and a small amount of-NH groups on the surface2A group. Fig. 7 is a time-dependent change curve of the fluorescence intensity of the yellow fluorescent carbon quantum dot obtained in this example at an emission wavelength of 568nm, which shows that the yellow fluorescent carbon quantum dot has good fluorescence stability in an ethanol solution.
According to the yellow fluorescent carbon quantum dot prepared by the implementation method, the reaction time is 2 hours at 180 ℃, in the embodiment, 2,4, 6-trihydroxybenzoic acid is used as a carbon source, m-phenylenediamine is used as a nitrogen source, a metal tin compound is used as a catalyst, and nitrogen atoms are doped into the carbon quantum dot, so that the light-emitting wavelength is red-shifted to a yellow light-emitting region, and the light-emitting efficiency of the carbon quantum dot is improved; in the embodiment, the metallic tin compound is used as the catalyst, so that the synthesis time of the carbon quantum dots is greatly shortened, and the synthesis cost of the carbon quantum dots is greatly reduced; the synthesis time is shortened by more than 50% compared with the time reported by the literature, and the quantum efficiency of the yellow carbon quantum dot synthesized in 2 hours can reach 38%.
Example two:
this embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, a preparation method of nitrogen-doped yellow carbon quantum dots, which synthesizes yellow carbon quantum dots by using 2,4, 6-trihydroxybenzoic acid as a carbon source, m-phenylenediamine as a nitrogen source, and a metallic tin salt as a catalyst and adopting a solvothermal method, includes the following steps:
a. weighing 1mmol of SnCl4·5H2Dissolving O and 1mmol of 2,4, 6-trihydroxybenzoic acid in 15mL of anhydrous ethanol, and heating to 40 ℃ under magnetic stirring to obtainA carbon source reactant solution; dissolving 2mmol of m-phenylenediamine in 5mL of absolute ethanol to form a nitrogen source reactant solution; dropwise adding the carbon source reactant solution into a nitrogen source reactant solution, and adjusting the pH value of the solution to 6; stirring at 40 deg.C for 60 min to mix the solution uniformly;
b. putting the uniformly mixed solution into a polytetrafluoroethylene reaction kettle, reacting for 2 hours at 160 ℃, and naturally cooling to room temperature to obtain a product solution;
c. and (3) performing centrifugal separation treatment on the product solution at the speed of 10000 r/min to remove tin oxide nanoparticles generated by the reaction, dialyzing for 1 day by using a membrane with the molecular weight of 3500Da, and removing small molecular substances, thereby obtaining the nitrogen-doped yellow carbon quantum dot solution with the nitrogen-doped yellow carbon quantum dot concentration of 23 mg/mL.
According to the yellow fluorescent carbon quantum dot prepared by the implementation method, the reaction time is 2 hours at 160 ℃, in the embodiment, 2,4, 6-trihydroxybenzoic acid is used as a carbon source, m-phenylenediamine is used as a nitrogen source, a metal tin compound is used as a catalyst, and nitrogen atoms are doped into the carbon quantum dot, so that the light-emitting wavelength is red-shifted to a yellow light-emitting region, and the light-emitting efficiency of the carbon quantum dot is improved; in the embodiment, the metallic tin compound is used as the catalyst, so that the synthesis time of the carbon quantum dots is greatly shortened, and the synthesis cost of the carbon quantum dots is greatly reduced; the synthesis time is shortened by more than 50% compared with the time reported by the literature, and the quantum efficiency of the yellow carbon quantum dot synthesized in 2 hours can reach 16.4%.
Example three:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a preparation method of nitrogen-doped yellow carbon quantum dots, which synthesizes yellow carbon quantum dots by using 2,4, 6-trihydroxybenzoic acid as a carbon source, m-phenylenediamine as a nitrogen source, and a metallic tin salt as a catalyst and adopting a solvothermal method, includes the following steps:
a. weighing 1mmol of SnCl4·5H2Dissolving O and 1mmol of 2,4, 6-trihydroxybenzoic acid in 15mL of absolute ethanol, and heating to 40 ℃ under magnetic stirring to obtain a carbon source reactant solution; then 2mmol ofDissolving m-phenylenediamine in 5mL of absolute ethanol to form a nitrogen source reactant solution; dropwise adding the carbon source reactant solution into a nitrogen source reactant solution, and adjusting the pH value of the solution to 6; stirring at 40 deg.C for 60 min to mix the solution uniformly;
b. putting the uniformly mixed solution into a polytetrafluoroethylene reaction kettle, reacting for 2 hours at 200 ℃, and naturally cooling to room temperature to obtain a product solution;
c. and (3) performing centrifugal separation treatment on the product solution at the speed of 10000 r/min to remove tin oxide nanoparticles generated by the reaction, dialyzing for 1 day by using a membrane with the molecular weight of 3500Da, and removing small molecular substances, thereby obtaining the nitrogen-doped yellow carbon quantum dot solution with the nitrogen-doped yellow carbon quantum dot concentration of 23 mg/mL.
According to the yellow fluorescent carbon quantum dot prepared by the implementation method, the reaction time is 2 hours at 200 ℃,2, 4, 6-trihydroxybenzoic acid is used as a carbon source, m-phenylenediamine is used as a nitrogen source, a metal tin compound is used as a catalyst, and the nitrogen atom is doped in the carbon quantum dot, so that the light-emitting wavelength is red-shifted to a yellow light-emitting region, and the light-emitting efficiency of the carbon quantum dot is improved; in the embodiment, the metallic tin compound is used as the catalyst, so that the synthesis time of the carbon quantum dots is greatly shortened, and the synthesis cost of the carbon quantum dots is greatly reduced; the synthesis time is shortened by more than 50% compared with the time reported by a literature, and the quantum efficiency of the yellow carbon quantum dot synthesized in 2 hours can reach 18%.
Comparative example:
in this comparative example, a method for preparing a carbon quantum dot, in which 2,4, 6-trihydroxybenzoic acid was used as a carbon source, m-phenylenediamine was used as a nitrogen source, and a metal tin salt was used as a catalyst, and a solvothermal method was used to synthesize a composite carbon quantum dot, including the following steps:
a. weighing 1mmol of SnCl4·5H2Dissolving O and 1mmol of 2,4, 6-trihydroxybenzoic acid in 15mL of absolute ethanol, and heating to 40 ℃ under magnetic stirring to obtain a carbon source reactant solution; dissolving 2mmol of m-phenylenediamine in 5mL of absolute ethanol to form a nitrogen source reactant solution; dropwise adding the carbon source reactant solution into a nitrogen source reactant solution, and adjusting the pH value of the solution to 6;stirring at 40 deg.C for 60 min to mix the solution uniformly;
b. putting the uniformly mixed solution into a polytetrafluoroethylene reaction kettle, reacting for 2 hours at 140 ℃, and naturally cooling to room temperature to obtain a product solution;
c. and (3) performing centrifugal separation treatment on the product solution at the speed of 10000 r/min to remove tin oxide nanoparticles generated by the reaction, dialyzing for 1 day by using a membrane with the molecular weight of 3500Da, and removing small molecular substances to obtain the composite carbon quantum dot solution.
The composite carbon quantum dot is prepared by the method with the reaction time of 2 hours at 140 ℃.
The quantum efficiencies of the prepared carbon quantum dots of the above examples and comparative examples are compared with each other in table 1.
TABLE 1 Quantum efficiency for the synthesis of yellow carbon quantum dots at different reaction temperatures
| Comparative example | Example two | Example one | EXAMPLE III | |
| Temperature/. degree.C | 140 | 160 | 180 | 200 |
| Absolute fluorescence quantum efficiency | 4.1％ | 16.4％ | 38.0％ | 18.0％ |
As can be seen from table 1, the quantum efficiency of synthesizing the yellow carbon quantum dots is greater than 16% when the reaction is performed at 160 to 200 ℃ for 2 hours, and the quantum efficiency of synthesizing the yellow carbon quantum dots is only 4.1% when the reaction is performed at 140 ℃ for 2 hours. Therefore, the temperature condition is a key technical condition element of the present invention.
In the step a, the tin salt adopts SnCl4·5H2O、SnCl4、SnCl2·2H2O、SnCl2And SnF2Any one or a mixture of any more of the salts is used as a catalyst, so that the synthesis time of the carbon quantum dots is shortened, and the synthesis cost of the carbon quantum dots is greatly reduced.
As can be seen from the above examples, the particle size of the yellow carbon quantum dot fluorescent material prepared in the above examples is in the range of 3 to 6 nm. The yellow carbon quantum can emit bright yellow fluorescence under the excitation of light with the wavelength of 320-550 nm, and the fluorescence quantum efficiency can reach 38% at most. In the preparation method of the embodiment, 2,4, 6-trihydroxybenzoic acid is used as a carbon source, m-phenylenediamine is used as a nitrogen source, and tin salt is used as a catalyst, so that the synthesis time for synthesizing the yellow carbon quantum dots is greatly shortened, the absolute fluorescence quantum efficiency of the synthesized yellow carbon quantum dots reaches 38%, and the concentration is not lower than 23 mg/mL. The yellow carbon quantum dots prepared by the method of the above example have stable fluorescence performance in ethanol solution, and no decrease of fluorescence intensity is observed within 35 days. The preparation method greatly simplifies the synthesis process of synthesizing the yellow carbon quantum dots, improves the preparation efficiency and greatly reduces the preparation cost.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, as long as the purpose of the present invention is met, and the present invention shall fall within the protection scope of the present invention without departing from the technical principle and inventive concept of the present invention.
Claims (10)
1. A nitrogen-doped yellow carbon quantum dot is characterized in that: the particle size range of the fluorescent powder is 3-6 nm, and yellow fluorescence can be emitted under the excitation of light with the wavelength of 320-550 nm; the nitrogen-doped yellow carbon quantum dots are dispersed in an ethanol solution, and the fluorescence intensity is not reduced within 35 days.
2. The nitrogen-doped yellow carbon quantum dot of claim 1, wherein: the maximum excitation wavelength for the nitrogen-doped yellow carbon quantum dots to emit yellow fluorescence is 525 nm.
3. The nitrogen-doped yellow carbon quantum dot of claim 2, wherein: under the excitation of light of 336-525 nm, yellow fluorescence can be emitted.
4. The nitrogen-doped yellow carbon quantum dot of claim 1, wherein: the maximum emission wavelength of yellow fluorescence is 568 nm.
5. The nitrogen-doped yellow carbon quantum dot of claim 1, wherein: the surface of which is bonded with-COOH, -OH and-NH2A group.
6. A method for preparing nitrogen-doped yellow carbon quantum dots according to claim 1, wherein the method comprises the following steps: the method for synthesizing the yellow carbon quantum dots by using the solvothermal method and taking 2,4, 6-trihydroxybenzoic acid as a carbon source, m-phenylenediamine as a nitrogen source and metallic tin salt as a catalyst comprises the following steps:
a. according to the molar ratio of the metallic tin salt to the 2,4, 6-trihydroxybenzoic acid of 1: (1-2), dissolving a metal tin salt and 2,4, 6-trihydroxybenzoic acid in ethanol, and adding a certain amount of m-phenylenediamine to form a mixed solution; the mol ratio of the m-phenylenediamine to the 2,4, 6-trihydroxybenzoic acid is 1: (1-2); adjusting the pH value of the mixed solution to 4-6, and stirring for 30-60 minutes at 40-70 ℃ to uniformly mix the solution;
b. putting the uniformly mixed solution into a polytetrafluoroethylene reaction kettle, reacting for 2-4 hours at 160-200 ℃, and then cooling to room temperature to obtain a product solution;
c. and (3) carrying out centrifugal separation treatment on the product solution, removing tin oxide, dialyzing by using a membrane with the molecular weight of 3500Da for at least 1 day, and removing small molecular substances, thereby obtaining the nitrogen-doped yellow carbon quantum dots.
7. The method for preparing nitrogen-doped yellow carbon quantum dots according to claim 6, wherein the method comprises the following steps: the yellow carbon quantum dots with high fluorescence quantum efficiency are synthesized, and the highest absolute fluorescence quantum efficiency reaches 38%.
8. The method for preparing nitrogen-doped yellow carbon quantum dots according to claim 6, wherein the method comprises the following steps: in the step a, SnCl is adopted as the tin salt4·5H2O、SnCl4、SnCl2·2H2O、SnCl2And SnF2Any one salt or a mixed salt of any several salts; or dissolving 1-2 mmol of 2,4, 6-trihydroxybenzoic acid and tin salt in at least 20mL of ethanol.
9. The method for preparing nitrogen-doped yellow carbon quantum dots according to claim 6, wherein the method comprises the following steps: in the step b, the reaction is carried out at 160-180 ℃.
10. The method for preparing nitrogen-doped yellow carbon quantum dots according to claim 6, wherein the method comprises the following steps: in the step c, the concentration of the obtained nitrogen-doped yellow carbon quantum dot solution is not lower than 23 mg/mL.
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| 丁媛媛等: ""高效橘色荧光碳量子点的合成及其在细胞成像中的应用"", 《山西大学学报》 * |
| 顾雪娇等: ""氮掺杂黄色碳荧光量子点的制备与表征"", 《辽宁化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113607709A (en) * | 2021-08-10 | 2021-11-05 | 河北科技大学 | Application of fluorescent carbon quantum dots in naphthenic acid detection and naphthenic acid detection method |
| CN113607709B (en) * | 2021-08-10 | 2024-05-10 | 河北科技大学 | Application of fluorescent carbon quantum dot in detection of naphthenic acid and detection method of naphthenic acid |
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| CN112391163B (en) | 2022-11-18 |
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