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Preparation method of nitrogen-doped graphene

A nitrogen-doped graphene and precursor technology, applied in the field of nitrogen-doped graphene preparation, can solve problems such as environmental pollution, polluting products, and difficulty in mass production of nitrogen-doped graphene, and achieve excellent performance and appearance. uniform effect

Active Publication Date: 2014-12-24
QINGDAO HAIYUAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the CVD method needs to use a metal catalyst, which will pollute the product, and it is not easy to mass-produce nitrogen-doped graphene; the hydrothermal method needs to use a toxic reducing agent, which will pollute the environment

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0019] The first step, the specific steps of preparing the precursor are as follows: the precursor is prepared in the following way: get 1.1g citric acid and 28.9g melamine (molar ratio is 1: 40), add in 150ml of anhydrous methanol, at room temperature Stir at a rate of 1000r / min for 10min, put the sample into a probe-type ultrasonic processor, and ultrasonicate for 10min in an ice-water bath at a power of 20kHz and 400W. Take out the sample after ultrasonication, heat it in a water bath at 80°C and stir it at a rate of 1000r / min until the sample has no obvious liquid water, move it into a blast drying oven, and dry it at 80°C for 24h to obtain the desired precursor.

[0020] In the second step, the precursor calcination process is as follows: put the precursor sample obtained above into a 100×50×50 cm boat-shaped crucible, cover it, place it in a tube furnace, and heat it at 6°C / min under an inert gas atmosphere Calcined at 600°C for 2h at a heating rate of 7°C / min, then calc...

Embodiment 2

[0024] The first step, the specific steps of preparing the precursor are as follows: the precursor is prepared in the following way: get 1.2g citric acid and 23.8g melamine (molar ratio is 1:30), add in 130ml of anhydrous methanol, at room temperature Stir at a rate of 800r / min for 20min, put the sample into a probe-type ultrasonic processor, and ultrasonicate for 15min in an ice-water bath at a power of 20kHz and 300W. The sample after ultrasonication was taken out, heated in a water bath at 70°C and stirred at a rate of 800r / min until the sample had no obvious liquid water, then moved into a blast drying oven, and dried at 70°C for 36h to obtain the desired precursor.

[0025] In the second step, the precursor calcination process is as follows: put the precursor sample obtained above into a 100×50×50 cm boat-shaped crucible, cover it, place it in a tube furnace, and heat it at 4°C / min under an inert gas atmosphere Calcined at 550°C for 2.5h at a heating rate of 5°C / min, then...

Embodiment 3

[0029] The first step, the specific steps of preparing the precursor are as follows: the precursor is prepared in the following way: get 1.4g citric acid and 18.6g melamine (molar ratio is 1:20), add in 100ml of anhydrous methanol, at room temperature Stir at a rate of 600r / min for 30min, put the sample into a probe-type ultrasonic processor, and ultrasonicate for 20min in an ice-water bath at a power of 20kHz and 200W. Take out the sample after ultrasonication, heat it in a water bath at 60°C and stir it at a speed of 600r / min until the sample has no obvious liquid water, move it into a blast drying oven, and dry it at 60°C for 48h to obtain the desired precursor.

[0030] In the second step, the precursor calcination process is as follows: put the precursor sample obtained above into a 100×50×50 cm boat-shaped crucible, cover it, place it in a tube furnace, and heat it at 2°C / min under an inert gas atmosphere Calcined at 500°C for 3h at a heating rate of 3°C / min, then calcin...

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Abstract

The invention relates to a preparation method of nitrogen-doped graphene. The preparation method comprises the following steps: adding raw materials of citric acid and melamine into methanol, stirring, performing ultrasonic treatment and drying to obtain a precursor, and calcining the precursor in a tubular furnace by two stages to finally obtain the nitrogen-doped grapheme. Compared with the prior art, the preparation method has the following advantages: the raw materials are wide in source; the steps are simple; requirements on equipment are low; in the preparation process, a reducing agent is not required, so that environment pollution is low; the prepared nitrogen-doped graphene is thin in sheet, large in specific surface area, uniform in structure and good in reproducibility.

Description

technical field [0001] The invention relates to the field of preparation of nano-carbon materials, in particular to a preparation method of nitrogen-doped graphene. Background technique [0002] Graphene is a carbon atom with sp 2 Carbon materials with a single-layer two-dimensional atomic structure composed of hybrid-connected monoatomic layers have been receiving scientific attention in recent years because of their extraordinary physical and electrochemical properties, such as high specific surface area, high electrical conductivity, and high mechanical strength. widespread attention in the world. Theoretical studies have shown that nitrogen doping can change the electronic structure and chemical properties of graphene, making it have n-type semiconductor properties, thereby expanding its applications in the fields of optics, electricity, and magnetism. [0003] At present, the commonly used methods for preparing nitrogen-doped graphene mainly include chemical vapor dep...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 朱申敏廖永亮张荻孙治华朱呈岭娄湘虹
Owner QINGDAO HAIYUAN IND
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