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Preparation method of nitrogen doped carbon based quantum dot

A technology of carbon-based quantum dots and nitrogen doping, which is applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of less waste liquid discharge, environmental protection, influence on the purity of synthesized carbon-based quantum dots, and short reaction time. It is easy to achieve The effects of purification, short preparation cycle and cheap raw materials

Inactive Publication Date: 2015-12-23
CHENGDU SCI & TECH DEV CENT CHINA ACAD OF ENG PHYSICS
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Problems solved by technology

On the one hand, comparing the preparation methods of carbon-based quantum dots, it is found that the microwave-assisted method not only requires simple equipment and short reaction time, but also has less waste liquid discharge, which is beneficial to environmental protection. Therefore, the microwave-assisted reaction method is an effective preparation method. , but on this basis, it is necessary to solve the problem of the influence of external absorbing materials on the purity of synthesized carbon-based quantum dots

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  • Preparation method of nitrogen doped carbon based quantum dot
  • Preparation method of nitrogen doped carbon based quantum dot
  • Preparation method of nitrogen doped carbon based quantum dot

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preparation example Construction

[0038] Further, the preparation method of nitrogen-doped carbon-based quantum dots comprises the following steps:

[0039] (1) Mix citric acid and imidazole compounds uniformly at a molar ratio of 1:0.5 to 1:12, wherein citric acid is a carbon source, and imidazole compounds are a nitrogen source.

[0040] (2) Heat the mixed material in step 1 with a microwave higher than 100W for 1-15 minutes to obtain a brown-black solid containing carbon-based quantum dots. According to the selection and adjustment of the reaction raw materials, the color of the carbon-based quantum dots obtained by microwave carbonization may be different, but this does not affect the realization of the purpose of the invention. Preferably, in order to facilitate the microwave treatment, the mixed material can be selected to be placed in a microwave oven for microwave treatment, and the microwave energy required for controlling the reaction material per unit volume (per liter) is not less than 1000KJ, and ...

Embodiment 1

[0047] Take 3g of citric acid and 0.9378g of imidazole solids (the molar ratio of citric acid and imidazole is 1:1) and put them in a beaker, stir them with a glass rod for physical mixing, put the mixed citric acid and imidazole directly in the microwave oven, set the microwave oven The power is 500W, and the reaction time is 3 minutes. After the reaction is completed, a brown-black solid is obtained, which contains the target nitrogen-doped carbon-based quantum dots.

[0048] Further, the product is purified. Add secondary water to the brown-black solid beaker, ultrasonically disperse for 30 minutes, vacuum filter the solution, and rinse with secondary water several times to remove unreacted citric acid and imidazole soluble in water, and obtain nitrogen-doped carbon-based Quantum dot filter cake. Finally, the filter cake was dried in a vacuum oven at 60°C for 1 hour to obtain pure nitrogen-doped carbon-based quantum dot solids.

Embodiment 2

[0050] Take 3g of citric acid and 2.8594g of imidazole solids (the molar ratio of citric acid and imidazole is 1:3) and put them in a beaker, stir them with a glass rod for physical mixing, put the mixed citric acid and imidazole directly in the microwave oven, set the microwave oven The power is 500W, and the reaction time is 3min. After the reaction is completed, a brown-black solid is obtained. Add secondary water to the beaker, ultrasonically disperse for 30 minutes, vacuum filter the solution, and rinse with secondary water several times to remove unreacted citric acid and imidazole soluble in water, and obtain nitrogen-doped carbon-based quantum dot filter cake. Finally, the filter cake was dried in a vacuum oven at 60°C for 1 hour to obtain pure nitrogen-doped carbon-based quantum dot solids. The UV absorption spectrum and fluorescence emission spectrum were tested as follows: figure 2 with image 3 , the results of specific nitrogen content and fluorescence luminous...

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Abstract

The invention provides a preparation method of a nitrogen doped carbon based quantum dot. According to the method, a cheap carbon source and nitrogen source are directly mixed, and then the mixture is carbonized by microwaves to prepare nitrogen doped carbon based quantum dots. In the prepared nitrogen doped carbon base quantum dot, nitrogen exists on the surface and skeleton structure of carbon based quantum dot in four chemical states: amino group, pyridine, pyrrole, and nitrogen-containing four-membered ring; furthermore, nitrogen chemical state relative contents and optical characteristics are adjustable; the prepared nitrogen doped carbon based quantum dot has the advantages of high fluorescence radiation efficiency and good catalytic effect, and the performance of the quantum dot can be further improved through modification, and the modified quantum dot can be applied to the fields such as catalysis, and the like. Moreover, in the preparation process, the nitrogen source and carbon source are directly mixed and carbonized, no wave absorbing material is needed, and the whole preparation process is simple and quick. The obtained carbon based quantum dot is insoluble in water, so the separation and purification of carbon based quantum dot can be completed in a short time, the yield is high, and the preparation method has an important meaning for production, application, and promotion of carbon based quantum dot.

Description

technical field [0001] The invention belongs to the field of nanometer material science, and specifically relates to a method for synthesizing nitrogen-doped carbon-based nanoparticles in one step by using a microwave-assisted method. Background technique [0002] In recent years, carbon nanomaterials composed of carbon elements have been continuously discovered, and its low toxicity or even non-toxicity makes it a hot material for technological innovation in the 21st century. Carbon-based nanoparticles (carbon-based quantum dots) were discovered by Sun in 2004 as a new type of carbon nanomaterial. It not only has the excellent luminescence performance of semiconductor quantum dots: it has a wide and continuous excitation spectrum, and can realize the characteristics of one-way excitation and multiple emission. ; The emission wavelength span is large, extending from the visible light region to the near-infrared light region; the fluorescence stability is high, and the biocom...

Claims

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Application Information

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IPC IPC(8): C09K11/65
Inventor 刘焕明黄家伟王群王聪唐昶宇赵云梅军
Owner CHENGDU SCI & TECH DEV CENT CHINA ACAD OF ENG PHYSICS
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