Nitrogen-doped porous graphene and a preparation method thereof

A porous graphene and nitrogen doping technology, applied in the field of carbon materials, can solve the problems of cumbersome process, harsh reaction conditions, low nitrogen doping amount, etc., and achieve the effects of simple process, short production cycle and large specific surface area.

Active Publication Date: 2014-10-22
太湖县市场监督检验所(太湖县功能膜检测研究院)
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Problems solved by technology

At present, these methods have the following disadvantages: chemical vapor deposition method, ammonia source pyrolysis method, nitrogen plasma discharge method, arc discharge method, etc. have the disadvantages of low nitrogen doping amount and multiple preparation procedures; liquid phase nitrogen doping method although nitrogen doping The amount can reach 16.4%, which may involve the dangerous raw material Li 3 N, the reaction conditions are relatively harsh
These methods usually require special equipment, cumbersome process, low efficiency, involve hazardous chemicals, and require substrates, etc.

Method used

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  • Nitrogen-doped porous graphene and a preparation method thereof

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[0017] The preparation method of nitrogen-doped porous graphene provided by the invention comprises:

[0018] Heating the mixture of nitrogen source and organic salt or organic acid and salt to 400-1600°C in a non-oxidizing atmosphere to obtain a mixture of nitrogen-doped porous graphene and metal oxide;

[0019] removing metal oxides in the mixture to obtain nitrogen-doped porous graphene;

[0020] Wherein, the nitrogen source is selected from one or more of imidazole compounds, pyridine compounds and triazole compounds;

[0021] Wherein, the organic salt is selected from magnesium, calcium, strontium, barium, cobalt, nickel, manganese, iron, zinc, aluminum, indium or bismuth citrate, gluconate, tartrate, threonate, carbon atom One or more of n-alkyl fatty acid salts and oleic acid salts whose number is 8-24;

[0022] Wherein, the organic acid is selected from one or more of citric acid, gluconic acid, tartaric acid, threonic acid, n-alkyl fatty acids with 8 to 24 carbon at...

Embodiment 1

[0037] Embodiment 1. Weigh 10 grams of ferric oleate and 2-methylimidazole and mix evenly, and put it into a magnetic boat, then use a tube furnace to heat up to 1200 ° C at a rate of 6 ° C / min in argon, Heated at 1200°C for 6 hours to obtain a mixture of nitrogen-doped porous graphene and iron oxide, washed with 10 ml of 37% concentrated hydrochloric acid at 50°C for 4 hours, and filtered to dryness to obtain in-situ nitrogen-doped porous graphene Graphene. According to elemental analysis, the nitrogen content of the nitrogen-doped porous graphene is 2.3%.

Embodiment 2

[0038] Example 2. After weighing 10 grams of magnesium citrate and 2 grams of benzimidazole and mixing them uniformly, put them into a magnetic boat, and then use a tube furnace to raise the temperature to 700°C at a rate of 4°C / min in argon. Heated at 700°C for 2 hours to obtain a mixture of nitrogen-doped porous graphene and magnesium oxide, washed with 10 ml of 37% concentrated hydrochloric acid at 50°C for 4 hours, and filtered to dryness to obtain nitrogen-doped porous graphene . According to elemental analysis, the nitrogen content of the nitrogen-doped porous graphene is 7.3%.

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Abstract

The invention relates to a nitrogen-doped porous graphene and a preparation method thereof. The preparation method comprises the following steps: heating a mixture of a nitrogen source and organic salts or organic acids and salts to 400-1600 DEG C under non-oxidizing atmosphere, to obtain a nitrogen-doped porous graphene and metal oxide mixture; removing the metal oxide in the mixture to obtain the nitrogen-doped porous graphene. The in-situ nitrogen-doped porous graphene having the advantages of being porous, large in specific surface area and the like can be prepared by heating the mixture of nitrogen source and organic salts or organic acids and salts under non-oxidizing atmosphere through utilizing the conception that organic salts are utilized to carbonize graphene, inorganic oxide is nucleated and a nitrogen source is pyrolyzed to generate activated nitrogen. The preparation method is simple in technology, free from needing special equipment, free from non-involving dangerous chemical products, short in production period and capable of doping nitrogen in situ. The prepared nitrogen-doped porous graphene can be applied in the fields of electric catalysis, a fuel battery catalyst, super capacitors, lithium ion batteries and the like.

Description

technical field [0001] The invention relates to the technical field of carbon materials, in particular to a nitrogen-doped porous graphene and a preparation method thereof. Background technique [0002] Since Geim et al. successfully prepared single-layer graphene in 2004, graphene has attracted widespread attention due to its excellent physical and chemical properties. Doping nitrogen atoms can induce the formation of high local charge / spin density on the surface of graphene to improve its chemical activity, making it transition from metallic properties to semiconducting properties. These characteristics make it an important functional graphene in electrocatalysis , fuel cell catalysts, supercapacitors and lithium-ion batteries and other fields have great application value. [0003] The preparation methods of nitrogen-doped graphene in the prior art include: flame method, arc discharge method, chemical vapor deposition method, ammonia source pyrolysis, plasma nitriding, et...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 马建民毛玉华
Owner 太湖县市场监督检验所(太湖县功能膜检测研究院)
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