CN111470493A - Preparation method and application of graphene quantum dots - Google Patents
Preparation method and application of graphene quantum dots Download PDFInfo
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- CN111470493A CN111470493A CN201910980252.8A CN201910980252A CN111470493A CN 111470493 A CN111470493 A CN 111470493A CN 201910980252 A CN201910980252 A CN 201910980252A CN 111470493 A CN111470493 A CN 111470493A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 30
- 239000002096 quantum dot Substances 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 9
- 238000010907 mechanical stirring Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 4
- 239000002041 carbon nanotube Substances 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 238000004146 energy storage Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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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
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- Physics & Mathematics (AREA)
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Abstract
The invention belongs to the field of graphene products, and particularly relates to a preparation method and application of graphene quantum dots. The invention provides a preparation method of graphene quantum dots, which comprises the following steps: dispersion, laser irradiation and purification. The invention also provides an application of the graphene quantum dot product prepared by the preparation method in the field of catalyst preparation. In the technical scheme provided by the invention, the preparation method of the graphene quantum dots is simple and convenient, other substances are not required to be introduced except for a solvent, and the prepared graphene quantum dots are high in purity and good in quality. The preparation method and the application of the graphene quantum dot provided by the invention solve the technical defects of complicated preparation and poor product quality of the preparation method of the graphene quantum dot in the prior art.
Description
Technical Field
The invention belongs to the field of graphene products, and particularly relates to a preparation method and application of graphene quantum dots.
Background
Graphene (Graphene) is a polymer made of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future.
Graphene Quantum Dots (GQDs) are zero-dimensional few-layer Graphene materials, and are at the nanometer level in three dimensions, so that GQDs exhibit some unique properties, such as: strong quantum confinement effects and edge effects. The GQDs also have good electronic conductivity and up-conversion luminescence characteristics, and the GQDs have the characteristics of no toxicity, low raw material price and the like, so that the GQDs have wide application prospects in application, for example, when zero-dimensional graphene quantum dots and two-dimensional nanosheets are combined, the quantum dots can be used as active sites to improve the catalytic activity of the catalyst.
In the prior art, when the graphene quantum dots are prepared, the preparation method is complex, auxiliaries such as a stabilizer need to be added, and after the reaction is completed, the auxiliaries are removed by an extraction method, the preparation steps are complex, and the auxiliaries cannot be completely removed, so that certain influence is caused on the quality of the prepared graphene quantum dots.
Therefore, a preparation method and an application of the graphene quantum dot are developed to solve the technical defects of complicated preparation and poor product quality of the preparation method of the graphene quantum dot in the prior art, and the problem to be solved by the technical staff in the field is urgently solved.
Disclosure of Invention
In view of this, the invention provides a preparation method of graphene quantum dots and an application thereof, which are used for solving the technical defects that the preparation method of graphene quantum dots in the prior art is complicated in preparation and poor in product quality.
The invention provides a preparation method of graphene quantum dots, which comprises the following steps:
step one, dispersing: dispersing carbon powder in a solvent to obtain a first product;
step two, laser irradiation: carrying out laser irradiation treatment on the first product to obtain a second product;
step three, purification: and centrifuging the second product and collecting the supernatant to obtain the graphene quantum dot product.
Preferably, in the first step, the carbon powder is selected from: any one or more of natural crystalline flake graphite, artificial crystalline flake graphite, carbon nanotubes and graphene.
Preferably, in the first step, the feeding ratio of the carbon powder to the solvent is 1 (0.5-2) g/ml.
Preferably, in step one, the solvent is selected from: any one or more of water, N-methylpyrrolidone, N-dimethylformamide, ethanol and isopropanol.
Preferably, in the first step, the dispersing method is mechanical stirring dispersing or ultrasonic dispersing.
Preferably, the stirring speed of the mechanical stirring is 500-1000 r/min, the temperature of the mechanical stirring is room temperature, and the time of the mechanical stirring is 0.5-1 h.
Preferably, in the second step, the wavelength of the laser beam irradiated by the laser is 10-760 nm, the energy irradiated by the laser is 200-500 mJ, the pulse frequency irradiated by the laser is 10-100 Hz, and the time irradiated by the laser is 1-3 h.
Preferably, in the third step, the rotating speed of the centrifugation is 8000-12000 r/min, and the time of the centrifugation is 20-60 min.
The invention also provides an application of the graphene quantum dot product prepared by the preparation method in the fields of catalyst preparation, energy storage devices and biomedicine.
In summary, the present invention provides a preparation method of graphene quantum dots, the preparation method comprising: dispersion, laser irradiation and purification. The invention also provides an application of the graphene quantum dot product prepared by the preparation method in the field of catalyst preparation. In the technical scheme provided by the invention, the preparation method of the graphene quantum dots is simple and convenient, other substances are not required to be introduced except for a solvent, and the prepared graphene quantum dots are high in purity and good in quality. The preparation method and the application of the graphene quantum dot provided by the invention solve the technical defects of complicated preparation and poor product quality of the preparation method of the graphene quantum dot in the prior art.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic flow chart of a preparation method of graphene quantum dots provided by the present invention;
fig. 2 is a schematic view of the graphene quantum dots in an electron microscope viewing field in example 5.
Detailed Description
The invention provides a preparation method and application of graphene quantum dots, and aims to overcome the technical defects that the preparation method of the graphene quantum dots in the prior art is complicated and the product quality is poor.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to illustrate the present invention in more detail, the following describes a preparation method and an application of the graphene quantum dot provided by the present invention in detail with reference to examples.
Example 1
5mg of carbon powder was dispersed in 10ml of water to obtain the first product 1. In the embodiment, the carbon powder is natural crystalline flake graphite; the dispersing method comprises the following steps: mechanically stirring at room temperature at a stirring speed of 500r/min for 1 h.
Carrying out laser irradiation treatment on the first product 1 to obtain a second product 1; the wavelength of the laser beam irradiated with the laser was 10nm, the energy of the laser irradiation was 200mJ, the pulse frequency of the laser irradiation was 60Hz, and the time of the laser irradiation was 3 h.
And centrifuging the second product 1 for 40min at the rotating speed of 11000r/min, and collecting supernate after centrifugation to obtain the graphene quantum dot product.
Example 2
10mg of carbon powder was dispersed in 10ml of N-methylpyrrolidone to obtain the first product 2. In the embodiment, the carbon powder is artificial flake graphite; the dispersing method comprises the following steps: mechanically stirring at room temperature at a stirring speed of 500r/min for 0.8 h.
Carrying out laser irradiation treatment on the first product 2 to obtain a second product 2; the wavelength of the laser beam irradiated by the laser was 220nm, the energy of the laser irradiation was 250mJ, the pulse frequency of the laser irradiation was 70Hz, and the time of the laser irradiation was 2.5 h.
And centrifuging the second product 2 at the rotating speed of 8000r/min for 50min, and collecting supernate after centrifugation to obtain the graphene quantum dot product.
Example 3
15mg of carbon powder was dispersed in 10ml of N, N-dimethylformamide to obtain the first product 3. In the present embodiment, the carbon powder is a carbon nanotube; the dispersing method comprises the following steps: mechanically stirring at room temperature at a stirring speed of 700r/min for 1 h.
Carrying out laser irradiation treatment on the first product 3 to obtain a second product 3; the wavelength of the laser beam irradiated by the laser was 560nm, the energy of the laser irradiation was 300mJ, the pulse frequency of the laser irradiation was 50Hz, and the time of the laser irradiation was 2 h.
And centrifuging the second product 3 at the rotating speed of 8500r/min for 60min, and collecting supernate after centrifugation to obtain the graphene quantum dot product.
Example 4
20mg of carbon powder was dispersed in 10ml of ethanol to obtain a first product 4. In the present embodiment, the carbon powder is a carbon nanotube; the dispersing method comprises the following steps: mechanically stirring at the room temperature at the stirring speed of 800r/min for 0.5 h.
Carrying out laser irradiation treatment on the first product 4 to obtain a second product 4; the wavelength of the laser beam irradiated with the laser was 760nm, the energy of the laser irradiation was 350mJ, the pulse frequency of the laser irradiation was 100Hz, and the time of the laser irradiation was 1.5 h.
And centrifuging the second product 4 at a rotating speed of 12000r/min for 30min, and collecting supernate after centrifugation to obtain the graphene quantum dot product.
Example 5
25mg of carbon powder was dispersed in 15ml of isopropanol to obtain a first product 5. In the present embodiment, the carbon powder is graphene; the dispersing method comprises the following steps: mechanically stirring at room temperature at a stirring speed of 1000r/min for 0.5 h.
Carrying out laser irradiation treatment on the first product 5 to obtain a second product 5; the wavelength of the laser beam irradiated with the laser was 340nm, the energy of the laser irradiation was 400mJ, the pulse frequency of the laser irradiation was 30Hz, and the time of the laser irradiation was 1 h.
And centrifuging the second product 5 at the rotating speed of 10000r/min for 20min, and collecting supernate after centrifugation to obtain the graphene quantum dot product.
Example 6
This example is a specific example for measuring the dispersion effect of the graphene quantum dots prepared in examples 1 to 5.
The obtained graphene quantum dots are observed under an electron microscope, and specifically, refer to fig. 2. As can be seen from fig. 2, the graphene quantum dots obtained by the preparation method are uniformly dispersed and have uniform particle size distribution. The technical scheme provided by the invention has the advantages that the graphene quantum dots are high in purity and good in quality, the preparation method is simple, convenient and quick, no impurities except a solvent are introduced, and the graphene quantum dots can be widely applied to the fields of catalyst preparation, energy storage devices and biomedicine.
In summary, the present invention provides a preparation method of graphene quantum dots, the preparation method comprising: dispersion, laser irradiation and purification. The invention also provides an application of the graphene quantum dot product prepared by the preparation method in the field of catalyst preparation. In the technical scheme provided by the invention, the preparation method of the graphene quantum dots is simple and convenient, other substances are not required to be introduced except for a solvent, and the prepared graphene quantum dots are high in purity and good in quality. The preparation method and the application of the graphene quantum dot provided by the invention solve the technical defects of complicated preparation and poor product quality of the preparation method of the graphene quantum dot in the prior art.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A preparation method of graphene quantum dots is characterized by comprising the following steps:
step one, dispersing: dispersing carbon powder in a solvent to obtain a first product;
step two, laser irradiation: carrying out laser irradiation treatment on the first product to obtain a second product;
step three, purification: and centrifuging the second product and collecting the supernatant to obtain the graphene quantum dot product.
2. The method as claimed in claim 1, wherein in step one, the carbon powder is selected from the group consisting of: any one or more of natural crystalline flake graphite, artificial crystalline flake graphite, carbon nanotubes and graphene.
3. The preparation method according to claim 1, wherein in the first step, the feeding ratio of the carbon powder to the solvent is 1 (0.5-2) mg/ml.
4. The method according to claim 1, wherein in step one, the solvent is selected from the group consisting of: any one or more of water, N-methylpyrrolidone, N-dimethylformamide, ethanol and isopropanol.
5. The method according to claim 1, wherein in the first step, the dispersing method is mechanical stirring dispersing or ultrasonic dispersing.
6. The preparation method according to claim 5, wherein the stirring speed of the mechanical stirring is 500 to 1000r/min, the temperature of the mechanical stirring is room temperature, and the time of the mechanical stirring is 0.5 to 1 h.
7. The method according to claim 1, wherein in the second step, the wavelength of the laser beam irradiated by the laser is 10 to 760nm, the energy of the laser irradiation is 200 to 500mJ, the pulse frequency of the laser irradiation is 10 to 100Hz, and the time of the laser irradiation is 1 to 3 hours.
8. The preparation method according to claim 1, wherein in the third step, the rotation speed of the centrifugation is 8000-12000 r/min, and the time of the centrifugation is 20-60 min.
9. The graphene quantum dot product prepared by the preparation method of any one of claims 1 to 8 is applied to the fields of catalyst preparation, energy storage devices and biomedicine.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113308172A (en) * | 2021-06-08 | 2021-08-27 | 南京工程学院 | Preparation and use method of composite anticorrosive paint for cable-stayed bridge inhaul cable |
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| CN113308172A (en) * | 2021-06-08 | 2021-08-27 | 南京工程学院 | Preparation and use method of composite anticorrosive paint for cable-stayed bridge inhaul cable |
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