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Preparation method of nitrogen-doped fluorescent carbon dots

A technology of fluorescent carbon dots and nitrogen doping, applied in the field of preparation of nitrogen doped fluorescent carbon dots, can solve the problems of low product yield, uncontrollable size, and poor crystallinity of carbon dots

Active Publication Date: 2016-05-18
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method generally has a high fluorescence quantum yield of carbon dots, and the preparation process is easy to operate, but the prepared carbon dots have poor crystallinity, uncontrollable size, and low product yield.

Method used

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  • Preparation method of nitrogen-doped fluorescent carbon dots
  • Preparation method of nitrogen-doped fluorescent carbon dots
  • Preparation method of nitrogen-doped fluorescent carbon dots

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Crush and grind the anthracite, sieve it with a 200-mesh screen, dry it in an oven at 100°C for 5 hours, cool to room temperature, weigh 504 mg of anthracite dried in the oven and place it in a 50 ml beaker, then add 20 ml of dimethylformamide , stir well, disperse the carbon source evenly and ultrasonically for 1.2h, then put the mixture in a 50ml hydrothermal kettle, and conduct a hydrothermal reaction at 180°C for 12h; After centrifuging at a speed of 9000rpm in a high-speed desktop centrifuge for 20 minutes, take the supernatant to obtain the hydrosol of fluorescent carbon dots; then place the hydrosol of fluorescent carbon dots in a rotary evaporation device, and after removing the organic solvent, the powdery Fluorescent carbon dots. Taking the fluorescent dye quinine sulfate as a reference, the quantum yield of the prepared fluorescent carbon dots reaches 12.5%, and taking anthracite as a reference, the product yield is 11.1wt.%. The morphology of the obtained t...

Embodiment 2

[0021] Grind the graphite powder, sieve it with a 200-mesh sieve, dry it in an oven at 110°C for 5 hours, cool to room temperature, weigh 504mg of the oven-dried graphite powder and place it in a 50ml beaker, then add 20ml of dimethyl formaldehyde Amide, stir well, disperse the carbon source evenly and sonicate for 1.2h, then put the mixture in a 50ml hydrothermal kettle, and conduct a hydrothermal reaction at 180°C for 12h; after the above reaction is completed, wait for the hydrothermal kettle to cool to room temperature, and take out the suspension After centrifuging at a speed of 9000rpm in a high-speed desktop centrifuge for 18 minutes, take the supernatant to obtain the hydrosol of fluorescent carbon dots; then place the hydrosol of fluorescent carbon dots in a rotary evaporation device to obtain powdered Fluorescent carbon dots. The resulting particle size distribution is figure 2 shown.

Embodiment 3

[0023] Crush and grind the bituminous coal, sieve it with a 200-mesh screen, dry it in an oven at 105°C for 6 hours, cool to room temperature, weigh 200 mg of bituminous coal dried in the oven and place it in a 50 ml beaker, then add 10 ml dimethylformamide , stir well, disperse the carbon source evenly and ultrasonically for 0.8h, then put the mixture in a 50ml hydrothermal kettle, and conduct a hydrothermal reaction at 80°C for 10h; After centrifuging at 8500rpm in a high-speed desktop centrifuge for 10 minutes, take the supernatant to obtain the hydrosol of fluorescent carbon dots; then place the hydrosol of fluorescent carbon dots in a rotary steamer, remove the organic solvent, and obtain powdered fluorescent carbon dots. Carbon dots.

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Abstract

The invention relates to the technical field of preparation of carbon nanomaterials and provides a preparation method of nitrogen-doped fluorescent carbon dots. The preparation method comprises the following steps: 1, a carbon source is broken, ground, sieved by a 200-mesh sieve and dried in an oven; 2, the carbon source dried by the oven is weighed and placed into a 50-ml beaker, then an organic solvent is added, and a mixture is stirred sufficiently and subjected to ultrasonic processing for 0.8-1.2 h; 3, the mixture prepared in the step 2 is placed in a 50-ml hydrothermal kettle to have a hydrothermal reaction for 2-12 h, and the temperature is controlled at 60-180 DEG C; 4, after step 3, a suspension is taken out and placed into a high-speed desk centrifuge, supernatant liquor is taken out after 10-20 min of centrifugation, and hydrosol of the fluorescent carbon dots is obtained; 5, the hydrosol, obtained in the step 4, of the fluorescent carbon dots is placed in rotary evaporation equipment, the organic solvent is removed, and the target product fluorescent carbon dots are prepared. The preparation method of the nitrogen-doped fluorescent carbon dots has the characteristics of green and environment-friendly reaction conditions, easiness in control and easiness in mass production and preparation and is expected to be widely applied to the fields of photoelectric devices, bio-imaging, detection, sensing and the like.

Description

technical field [0001] The invention relates to a method for preparing nitrogen-doped fluorescent carbon dots, and belongs to the technical field of carbon nanomaterial preparation. Background technique [0002] Carbon dots are fluorescent carbon particles composed of single-layer or few-layer graphene sheets with a particle size of less than 20 nm. It was first obtained from the lysate of carbon nanotubes by the University of South Carolina in 2004. extracted by-products. Studies have found that carbon dots have attracted widespread attention due to their excellent properties such as excellent fluorescence characteristics, good biocompatibility, low toxicity, good photostability, and no light flickering phenomenon. Fields such as sensing show great application potential. [0003] At present, the preparation methods of carbon dots are mainly divided into two categories: 1) "top-down" method, which generally uses harsh chemical reactions, such as arc discharge, laser ablati...

Claims

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Application Information

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IPC IPC(8): C09K11/65C01B31/02B82Y20/00B82Y40/00
CPCC09K11/0883C09K11/65
Inventor 邱介山李明宇于畅胡超王秀娜王玉伟
Owner DALIAN UNIV OF TECH
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