CN110885679A - White fluorescent carbon dots and preparation method thereof - Google Patents
White fluorescent carbon dots and preparation method thereof Download PDFInfo
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- CN110885679A CN110885679A CN201911094583.8A CN201911094583A CN110885679A CN 110885679 A CN110885679 A CN 110885679A CN 201911094583 A CN201911094583 A CN 201911094583A CN 110885679 A CN110885679 A CN 110885679A
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Abstract
The invention relates to a preparation method of white fluorescent carbon dots, which is characterized by comprising the following steps: step S1, preparation of a precursor I; step S2, preparation of a precursor II; step S3, preparation of a precursor III; step S4, preparing carbon dots; and step S5, preparing white fluorescence. The invention also discloses the white fluorescent carbon dots prepared by the preparation method of the white fluorescent carbon dots. The preparation method of the white fluorescent carbon dots disclosed by the invention is simple and easy to implement, the preparation efficiency and the finished product qualification rate are high, and the economic value, the social value, the ecological value and the popularization and application value are high; the prepared white fluorescent carbon dot has low toxicity, good biocompatibility, high fluorescence intensity, high storage stability and high fluorescence quantum yield, and effectively solves the technical problems of difficult doping of quantum dots and difficult preparation of white fluorescence in the prior art.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a white fluorescent carbon dot and a preparation method thereof.
Background
In recent years, quantum dots have been favored by a large number of researchers of nanomaterials as a latest carbon material due to its excellent optical properties and low biotoxicity. The quantum dots have excellent properties such as hydrophilicity, low cytotoxicity, chemical and light stability and the like, so that the quantum dots are widely concerned and applied in the fields of chemistry, biomedicine, sensing and optoelectronics.
The preparation of quantum dots is an important issue in the field of carbon material research. At present, the method is mainly divided into two categories: a bottom-up approach and a bottom-up approach. In addition, the doping of the heterocyclic elements can change the band structure and the surface functional group structure of the quantum dots to a great extent, so that the quantum dots have different optical properties. At present, researchers have prepared quantum dots with different fluorescence by various physical and chemical means. However, the quantum dots prepared by the methods have the problems of difficult doping, difficult preparation of white fluorescent quantum dots and the like, and the existing carbon quantum dots (carbon dots for short) still have the defect of low fluorescent quantum yield.
Chinese patent application CN103788402A discloses a novel water-soluble fluorescent material (i.e., carbon quantum dot) with a primary diameter of 5-10nm, which is prepared from soluble natural high molecular polymers containing amino groups such as gelatin or chitosan, and the preparation process can adopt various methods such as hydrothermal, microwave and ultrasonic, but the carbon quantum dot prepared by the method has low fluorescence intensity and fluorescence yield and poor storage stability.
Therefore, there is a need to develop a carbon quantum dot with low toxicity, good biocompatibility, high fluorescence intensity, stable storage and high fluorescence quantum yield, so as to solve the technical problems of difficult doping of quantum dots and difficult preparation of white fluorescence in the prior art.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a white fluorescent carbon dot and a preparation method thereof, wherein the method is simple and easy to implement, the preparation efficiency and the finished product qualification rate are high, and the economic value, the social value, the ecological value and the popularization and application value are high; the prepared white fluorescent carbon dot has low toxicity, good biocompatibility, high fluorescence intensity, stable storage and high fluorescence quantum yield, and effectively solves the technical problems of difficult doping of quantum dots and difficult preparation of white fluorescence in the prior art. The white fluorescent carbon dots synthesized by the method greatly improve the luminescence stability of the carbon dots, and the one-step in-situ doping method is used, so that the complex passivation treatment in the traditional doped quantum dot preparation process is effectively simplified, and the fluorescence stability of the quantum dots is greatly improved, so that the white fluorescent carbon dots have wide application prospects in more fields of luminescent devices, biological medicines and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a white fluorescent carbon dot is characterized by comprising the following steps:
step S1, preparation of precursor I: dissolving citric acid in an anhydrous alcohol solvent, and uniformly stirring to obtain a precursor I;
step S2, preparation of precursor II: dissolving o-phenylenediamine in absolute ethyl alcohol, and uniformly stirring to obtain a precursor II;
step S3, preparation of precursor III: dissolving a hydrogen peroxide solution in absolute ethyl alcohol, and uniformly stirring to obtain a precursor III;
step S4, preparation of carbon dots: uniformly mixing the precursor I prepared in the step S1, the precursor II prepared in the step S2 and the precursor III prepared in the step S3 according to the volume ratio of 1:1:1 to obtain a mixed material, transferring the mixed material into an inner container of a polytetrafluoroethylene hydrothermal reaction kettle for ultrasonic treatment for 25-35min, transferring the mixed material into a hydrothermal oven, heating to 180-190 ℃, preserving heat for 10-15h for hydrothermal reaction, and cooling to room temperature along with the oven to obtain carbon dots;
step S5, preparation of white fluorescence: the carbon dots prepared in step S4 were diluted with absolute ethanol and irradiated with UV light of 360-370nm to obtain white fluorescent carbon dots.
Further, in the step S1, the proportion of the citric acid and the anhydrous alcohol solvent is 18mg (15-20) mL.
Preferably, the anhydrous alcohol solvent is anhydrous ethanol.
Further, in the step S2, the ratio of the o-phenylenediamine to the anhydrous alcohol solvent is 108mg (15-20) mL.
Preferably, the hydrogen peroxide solution in step S3 has a concentration of 30% by mass.
Further, in the step S3, the volume ratio of the hydrogen peroxide to the absolute ethyl alcohol is (1-5): 15.
Further, the preparation principle of the white fluorescent carbon dot is as follows: in an ethanol solvent, under the catalytic action of hydrogen peroxide, citric acid and o-phenylenediamine are subjected to dehydration reaction to form a graphene-like structure, and the structure contains a large number of nitrogen and oxygen containing functional groups.
Further, the reaction equation of the dehydration reaction is:
another object of the present invention is to provide a white fluorescent carbon dot prepared according to the method for preparing a white fluorescent carbon dot.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the white fluorescent carbon dots and the preparation method thereof provided by the invention are simple and easy to implement, high in preparation efficiency and finished product qualification rate, and high in economic value, social value, ecological value and popularization and application value; the prepared white fluorescent carbon dot has low toxicity, good biocompatibility, high fluorescence intensity, stable storage and high fluorescence quantum yield, and effectively solves the technical problems of difficult doping of quantum dots and difficult preparation of white fluorescence in the prior art. The white fluorescent carbon dots synthesized by the method greatly improve the luminescence stability of the carbon dots, and the one-step in-situ doping method is used, so that the complex passivation treatment in the traditional doped quantum dot preparation process is effectively simplified, and the fluorescence stability of the quantum dots is greatly improved, so that the white fluorescent carbon dots have wide application prospects in more fields of luminescent devices, biological medicines and the like.
Drawings
FIG. 1 is an ultraviolet-visible absorption spectrum (inset is a fluorescence plot of quantum dots under 365 UV) of a carbon dot made in example 1;
FIG. 2 is a fluorescence emission spectrum of the carbon dot prepared in example 1;
fig. 3 is a TEM of the carbon dots made in example 1.
Detailed Description
The invention relates to a preparation method of white fluorescent carbon dots, which is characterized by comprising the following steps:
step S1, preparation of precursor I: dissolving citric acid in an anhydrous alcohol solvent, and uniformly stirring to obtain a precursor I;
step S2, preparation of precursor II: dissolving o-phenylenediamine in absolute ethyl alcohol, and uniformly stirring to obtain a precursor II;
step S3, preparation of precursor III: dissolving a hydrogen peroxide solution in absolute ethyl alcohol, and uniformly stirring to obtain a precursor III;
step S4, preparation of carbon dots: uniformly mixing the precursor I prepared in the step S1, the precursor II prepared in the step S2 and the precursor III prepared in the step S3 according to the volume ratio of 1:1:1 to obtain a mixed material, transferring the mixed material into an inner container of a polytetrafluoroethylene hydrothermal reaction kettle for ultrasonic treatment for 25-35min, transferring the mixed material into a hydrothermal oven, heating to 180-190 ℃, preserving heat for 10-15h for hydrothermal reaction, and cooling to room temperature along with the oven to obtain carbon dots;
step S5, preparation of white fluorescence: the carbon dots prepared in step S4 were diluted with absolute ethanol and irradiated with UV light of 360-370nm to obtain white fluorescent carbon dots.
Further, the proportion of the citric acid and the anhydrous alcohol solvent in the step S1 is 18mg (15-20) mL; the absolute alcohol solvent is absolute ethyl alcohol; in the step S2, the proportion of the o-phenylenediamine to the absolute alcohol solvent is 108mg (15-20) mL; the mass percentage concentration of the hydrogen peroxide solution in the step S3 is 30%; in the step S3, the volume ratio of the hydrogen peroxide to the absolute ethyl alcohol is (1-5): 15.
Further, the preparation principle of the white fluorescent carbon dot is as follows: in an ethanol solvent, under the catalytic action of hydrogen peroxide, citric acid and o-phenylenediamine are subjected to dehydration reaction to form a graphene-like structure, and the structure contains a large number of nitrogen and oxygen containing functional groups.
Further, the reaction equation of the dehydration reaction is:
another object of the present invention is to provide a white fluorescent carbon dot prepared according to the method for preparing a white fluorescent carbon dot.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the white fluorescent carbon dots and the preparation method thereof provided by the invention are simple and easy to implement, high in preparation efficiency and finished product qualification rate, and high in economic value, social value, ecological value and popularization and application value; the prepared white fluorescent carbon dot has low toxicity, good biocompatibility, high fluorescence intensity, stable storage and high fluorescence quantum yield, and effectively solves the technical problems of difficult doping of quantum dots and difficult preparation of white fluorescence in the prior art. The white fluorescent carbon dots synthesized by the method greatly improve the luminescence stability of the carbon dots, and the one-step in-situ doping method is used, so that the complex passivation treatment in the traditional doped quantum dot preparation process is effectively simplified, and the fluorescence stability of the quantum dots is greatly improved, so that the white fluorescent carbon dots have wide application prospects in more fields of luminescent devices, biological medicines and the like.
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto.
Example 1
Embodiment 1 provides a method for preparing a white fluorescent carbon dot, comprising the following steps:
step S1: dissolving 18mg of citric acid in 15mL of absolute ethanol to obtain a precursor I;
step S2: dissolving 108mg of o-phenylenediamine in 15mL of absolute ethanol to obtain a precursor II;
step S3: dissolving 3mL of 30% hydrogen peroxide in 15mL of absolute ethyl alcohol to obtain a precursor III;
step S4: and mixing the precursors III and II and the precursor 1 according to the ratio of 1:1, transferring the mixture into a polytetrafluoroethylene hydrothermal reaction liner of 50mL for ultrasonic treatment for 30min, transferring the mixture into a hydrothermal oven, heating to 180 ℃, preserving heat for 12h, carrying out hydrothermal reaction, and cooling to room temperature along with the oven to obtain carbon dots;
step S5: diluting the carbon dots by 4 times with absolute ethyl alcohol, and irradiating by using a 365nm ultraviolet lamp to obtain cold white fluorescence.
Fig. 1 shows a UV-Visa spectrum of a prepared carbon dot, in which the absorption peak at 293nm is a transition and the absorption peak at 380nm is a transition from C to N in the N functional group. The fluorescence emission spectrum is shown in FIG. 2, and a bimodal emission curve appears. The uv lamp emits intense white light under illumination, see inset in fig. 2. The particle size of the prepared carbon dots is 15-40 nm. The quantum yield was 65%.
Example 2
Embodiment 2 provides a method for preparing a white fluorescent carbon dot, which comprises the following steps:
step S1: dissolving 18mg of citric acid in 15mL of absolute ethanol to obtain a precursor I;
step S2: dissolving 108mg of o-phenylenediamine in 15mL of absolute ethanol to obtain a precursor II;
step S3: dissolving 1mL of 30% hydrogen peroxide in 15mL of absolute ethyl alcohol to obtain a precursor III;
step S4: and mixing the precursors III and II and the precursor 1 according to the ratio of 1:1, transferring the mixture into a polytetrafluoroethylene hydrothermal reaction liner of 50mL for ultrasonic treatment for 30min, transferring the mixture into a hydrothermal oven, heating to 180 ℃, preserving heat for 12h, carrying out hydrothermal reaction, and cooling to room temperature along with the oven to obtain carbon dots;
step S5: diluting the carbon dots by 3 times with absolute ethyl alcohol, and irradiating by using a 365nm ultraviolet lamp to obtain cold white fluorescence. The prepared carbon dot particles have the size of 5-20 nm. The quantum yield was 35%.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. A preparation method of a white fluorescent carbon dot is characterized by comprising the following steps:
step S1, preparation of precursor I: dissolving citric acid in an anhydrous alcohol solvent, and uniformly stirring to obtain a precursor I;
step S2, preparation of precursor II: dissolving o-phenylenediamine in absolute ethyl alcohol, and uniformly stirring to obtain a precursor II;
step S3, preparation of precursor III: dissolving a hydrogen peroxide solution in absolute ethyl alcohol, and uniformly stirring to obtain a precursor III;
step S4, preparation of carbon dots: uniformly mixing the precursor I prepared in the step S1, the precursor II prepared in the step S2 and the precursor III prepared in the step S3 according to the volume ratio of 1:1:1 to obtain a mixed material, transferring the mixed material into an inner container of a polytetrafluoroethylene hydrothermal reaction kettle for ultrasonic treatment for 25-35min, transferring the mixed material into a hydrothermal oven, heating to 180-190 ℃, preserving heat for 10-15h for hydrothermal reaction, and cooling to room temperature along with the oven to obtain carbon dots;
step S5, preparation of white fluorescence: the carbon dots prepared in step S4 were diluted with absolute ethanol and irradiated with UV light of 360-370nm to obtain white fluorescent carbon dots.
2. The method for preparing a white fluorescent carbon dot according to claim 1, wherein the ratio of the citric acid to the absolute alcohol solvent in step S1 is 18mg (15-20) mL.
3. The method of claim 1, wherein the absolute alcohol solvent is absolute ethanol.
4. The method for preparing a white fluorescent carbon dot according to claim 1, wherein the ratio of the o-phenylenediamine to the anhydrous alcohol solvent in step S2 is 108mg (15-20) mL.
5. The method of claim 1, wherein the hydrogen peroxide solution is used in step S3 at a concentration of 30 wt%.
6. The method of claim 5, wherein the volume ratio of hydrogen peroxide to absolute ethyl alcohol in step S3 is (1-5): 15.
7. A white fluorescent carbon dot prepared according to the method for preparing a white fluorescent carbon dot of claims 1 to 6.
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| TWI752859B (en) * | 2021-04-09 | 2022-01-11 | 臺南紡織股份有限公司 | Carbon nanodots fluorescent polymer, a method for preparing the same, and carbon nanodots fluorescent fibers |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI752859B (en) * | 2021-04-09 | 2022-01-11 | 臺南紡織股份有限公司 | Carbon nanodots fluorescent polymer, a method for preparing the same, and carbon nanodots fluorescent fibers |
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