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A kind of preparation method of nitrogen-doped graphene quantum dot material

A technology of graphene quantum dots and nitrogen doping, which is applied in the field of nanomaterials, can solve the problems of graphene quantum dot doping difficulties, unstable luminescence, etc., and achieve mass production, improve charge transport capabilities, and reduce costs.

Inactive Publication Date: 2021-01-12
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a stable nitrogen-doped graphene quantum dot material preparation method for the difficulties in doping graphene quantum dots and unstable luminescence in the prior art.

Method used

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  • A kind of preparation method of nitrogen-doped graphene quantum dot material
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  • A kind of preparation method of nitrogen-doped graphene quantum dot material

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Take 0.1g of network-shaped reduced graphene oxide, disperse it in 100ml of concentrated nitric acid with a mass percentage of 65%, stir it magnetically, heat the oil bath to 150°C while circulating water condenses, and react at a constant temperature for 12h; then remove the condensed water and continue to evaporate at a constant temperature for 2h; Cool to room temperature, then add ultrapure water for ultrasonic dispersion for 15 minutes; filter, and concentrate the filtrate to 10 mL by rotary evaporation, put it into a 3000Da dialysis bag for dialysis for 2 days; the obtained dialysate is again concentrated by rotary evaporation to obtain a high concentration of nitrogen-doped graphene quantum points; finally, vacuum freeze-drying at -50~-60°C for 10 h to obtain brown nitrogen-doped graphene quantum dots with a yield of 70%.

[0034] The particle size of the brown nitrogen-doped graphene quantum dots is about 8nm; the fluorescence emission color of the quantum dots i...

Embodiment 2

[0036] Take 0.1g of network-shaped reduced graphene oxide, disperse it in 100ml of concentrated nitric acid with a mass percentage of 65%, heat it in an oil bath under magnetic stirring to 150°C while circulating water condenses, and react at a constant temperature for 24 hours; then remove the condensed water and continue to evaporate at a constant temperature for 2 hours; Cool to room temperature, add ultrapure water to it for ultrasonic dispersion for 15min; filter, and concentrate the filtrate to 15mL by rotary evaporation; then put it into a 3000Da dialysis bag and dialyze for 1 day; the dialysate is again concentrated by rotary evaporation to obtain high-concentration nitrogen-doped graphene Quantum dots; finally, vacuum freeze-drying at -50~-60°C for 10 hours to obtain yellow nitrogen-doped graphene quantum dots. The yield was 54%.

[0037] The particle size of the yellow nitrogen-doped graphene quantum dots is about 5nm; the fluorescence emission color of the quantum d...

Embodiment 3

[0039] Take 0.1g of network reduced graphene oxide, disperse it in 100ml of concentrated nitric acid with a mass percentage of 65%, heat it in an oil bath under magnetic stirring to 150°C while circulating water condenses, and react at a constant temperature for 48h; then remove the condensed water and continue to evaporate at a constant temperature for 1.5h Cool to room temperature, add ultrapure water and ultrasonically disperse for 10min; filter, the filtrate is concentrated to 15mL by rotary evaporation, and put into a 3000Da dialysis bag for dialysis for 2 days; the dialysate is again concentrated by rotary evaporation to obtain high-concentration nitrogen-doped graphene quantum dots ; Finally, vacuum freeze-drying at -50~-60°C for 10 hours to obtain light yellow nitrogen-doped graphene quantum dots. The yield was 35%.

[0040] The particle size of the light yellow nitrogen-doped graphene quantum dots is about 4nm; the fluorescence emission color of the quantum dots under t...

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Abstract

The invention provides a stable method for preparing a nitrogen-doped graphene quantum dot material. The preparation method comprises the following steps: dispersing networked reduced graphene oxide in concentrated nitric acid, and heating in an oil bath to a temperature of 140-160 DEG C while magnetic stirring, and reacting at a constant temperature for 12-48 hours under circulating water condensation; removing circulating condensate water, continuously evaporating at the constant temperature for 2-3 hours, and cooling to a room temperature; adding ultrapure water for ultrasonic dispersion, filtering, performing rotary evaporation and concentration on the filtrate, and filling in a dialysis bag of 3000-8000Da to dialyze for 24-48 hours; and performing rotary evaporation and concentrationon the dialysate again, and performing vacuum freeze drying, thereby obtaining the nitrogen-doped graphene quantum dots. The luminous stability of the nitrogen-doped graphene quantum dot is improved to a certain degree, and complicated passivating treatment and mixed element doping processes in the traditional process of preparing the doped quantum dots are effectively simplified. Moreover, the charge transfer capacity of the quantum dots is effectively improved, and the application potential in more fields such as photoelectricity, biomedicine and the like is facilitated.

Description

technical field [0001] The invention relates to a method for preparing a graphene quantum dot material, in particular to a method for preparing a graphene quantum dot material through an aza network graphene material, and belongs to the technical field of nanometer materials. Background technique [0002] Since the Nobel Prize winner Geim et al. discovered graphene in 2004, graphene has become the most promising two-dimensional nanostructure material due to its outstanding advantages in various fields such as mechanics, electricity, optics, and heat. There are too many related studies on derivative materials. In recent years, graphene quantum dots have been developed as the latest member of the graphene family, and are favored due to their good water solubility, biocompatibility, low toxicity, and stable fluorescence; and because they inherit graphene The excellent performance also has quantum confinement effect and boundary effect, which greatly opens up the application pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19C01B32/194
CPCC01B2204/32
Inventor 莫尊理张红娟郭瑞斌冯航空刘振宇
Owner NORTHWEST NORMAL UNIVERSITY
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