Method for preparing nitrogen-doped graphene quantum dot material

A graphene quantum dot, nitrogen doping technology, applied in the field of nanomaterials, can solve the problems of unstable luminescence, difficult doping of graphene quantum dots, etc., to improve the charge transport capability, realize mass production, and strong fluorescence emission performance. Effect

Inactive Publication Date: 2018-04-06
NORTHWEST NORMAL UNIVERSITY
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  • 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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  • Method for preparing nitrogen-doped graphene quantum dot material
  • Method for preparing nitrogen-doped graphene quantum dot material
  • Method for preparing nitrogen-doped graphene quantum dot material

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Take 0.1g of network-like reduced graphene oxide, disperse it in 100ml of 65% by mass concentrated nitric acid, stir it magnetically, heat the oil bath to 150℃ while condensing the circulating water, 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 ultra-pure water and ultrasonically disperse for 15 minutes; filter, rotary evaporate and concentrate the filtrate to 10 mL, and put it into a 3000Da dialysis bag for dialysis for 2 days; the resulting dialysate is concentrated by rotary evaporation again to obtain high-concentration nitrogen-doped graphene quantum Dots; finally, vacuum freeze-drying at -50~-60℃ for 10h to obtain brown nitrogen-doped graphene quantum dots with a yield of 70%.

[0034] The particle size of brown nitrogen-doped graphene quantum dots is about 8nm; the fluorescence emission color of quantum dots under the irradiation of a 365nm ultra...

Embodiment 2

[0036] Take 0.1g of network-shaped reduced graphene oxide and disperse it in 100ml of 65% by mass concentrated nitric acid. Under magnetic stirring, the oil bath is heated to 150°C while circulating water is condensed and reacted at a constant temperature for 24h; then the condensed water is removed and the constant temperature evaporation is continued for 2h; Cool to room temperature, add ultrapure water and ultrasonically disperse for 15min; filter, and concentrate the filtrate by rotary evaporation to 15mL; then put it into a 3000Da dialysis bag for dialysis for 1 day; the dialysate is concentrated by rotary evaporation again to obtain high-concentration nitrogen-doped graphene Quantum dots; finally, vacuum freeze-drying at -50~-60℃ for 10h 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 fluorescent emission color of the quantum dots under the irradiation o...

Embodiment 3

[0039] Take 0.1g of network-shaped reduced graphene oxide and disperse it in 100ml of 65% by mass concentrated nitric acid. Under magnetic stirring, the oil bath is heated to 150°C while circulating water is condensed, reacting at a constant temperature for 48h; then the condensed water is removed and evaporation is continued at constant temperature for 1.5h ; Cool to room temperature, add ultra-pure water and ultrasonically disperse for 10 min; filter, rotary evaporate and concentrate the filtrate to 15 mL, and put it into a 3000Da dialysis bag for 2 days; the dialysate is concentrated by rotary evaporation again to obtain high-concentration nitrogen-doped graphene quantum dots ; Finally, vacuum freeze-drying at -50~-60℃ for 10h 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 fluorescent emission color of the quantum dots under the irradiation of ...

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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 graphene quantum dot materials, in particular to a method for preparing graphene quantum dot materials through aza network graphene materials, and belongs to the technical field of nano materials. Background technique [0002] Since the Nobel Prize winner Geim and others discovered graphene in 2004, graphene has become the most promising two-dimensional nanostructured material due to its outstanding advantages in various fields such as mechanics, electricity, optics, and heat. The research on related derivative materials is even more numerous. In recent years, graphene quantum dots have been developed as the latest member of the graphene family. They are favored due to their good water solubility, biocompatibility, low toxicity, and stable fluorescence; and because they are inheriting graphene The excellent performance also has quantum confinement effect and boundary effect, which greatly opens up the applica...

Claims

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Application Information

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Patent Type & Authority Applications(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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