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Three-dimensional porous nitrogen-doped graphene and preparation method and application thereof

A nitrogen-doped graphene, three-dimensional porous technology, applied in the direction of electrical components, battery electrodes, circuits, etc., can solve the problems of high preparation conditions, difficulty in large-scale production, and high synthesis cost, so as to improve electrocatalytic activity and activity , the effect of improving stability

Inactive Publication Date: 2017-07-25
佛山市利元合创科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be seen from this that the traditional preparation of nitrogen-doped graphene with three-dimensional porous structure is cumbersome and requires high preparation conditions. Due to the pollution of the environment due to the use of a large number of chemical reagents, especially toxic reagents, the synthesis cost is high and it is difficult to produce on a large scale.

Method used

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  • Three-dimensional porous nitrogen-doped graphene and preparation method and application thereof
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  • Three-dimensional porous nitrogen-doped graphene and preparation method and application thereof

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preparation example Construction

[0027] The invention provides a preparation method of three-dimensional porous nitrogen-doped graphene, comprising the following steps:

[0028] (1) mixing amino acid with transition metal salt and water to obtain a mixed solution;

[0029] (2) heating the mixed solution obtained in the step (1) to remove moisture under stirring to obtain a solid mixture;

[0030] (3) roasting the solid mixture obtained in the step (2) after grinding to obtain nitrogen-doped carbon powder;

[0031] (4) Grinding the nitrogen-doped carbon powder obtained in the step (3) and sequentially washing with acid, deionized water, absolute ethanol and drying to obtain three-dimensional porous nitrogen-doped graphene.

[0032] The invention mixes amino acid, transition metal salt and water to obtain a mixed solution.

[0033] The present invention does not have any special limitation on the source of the amino acid and the transition metal salt, and commercially available products well known to those sk...

Embodiment 1

[0061] (1) 1g of glycine will be mixed with different proportions of transition metal salt FeCl 3 ·6H 2 O mixed to obtain mixture 1 (glycine: FeCl 3 ·6H 2 The mass ratio of O is 1:1), mixture 2 (glycine:FeCl 3 ·6H 2 The mass ratio of O is 1:2) and mixture 3 (glycine:FeCl 3 ·6H 2 The mass ratio of O is 1:4); mixture 4 (glycine:FeCl 3 ·6H 2 The mass ratio of O is 1:6); mixture 5 (glycine:FeCl 3 ·6H 2 The mass ratio of O is 1:8); mixture 6 (glycine:FeCl 3 ·6H 2 The mass ratio of O is 1:10);

[0062] (2) Add 40 mL of deionized water to the six mixtures of step (1), and stir at room temperature;

[0063] (3) heating the solution in step (2) to 80° C. under stirring until the water is evaporated;

[0064](4) the product in step (3) is put into a quartz boat after being ground, then placed in a tube furnace, under N 2 Under the atmosphere, the temperature was raised to 950°C at a heating rate of 5°C / min, kept for 60 minutes, and then lowered to room temperature at a coo...

Embodiment 2

[0067] (1) Mix 1g glycine with 2g transition metal salt CoCl 2 ·6H 2 O mixed;

[0068] (2) Add 40 mL of deionized water to the mixture in step (1), and stir at room temperature;

[0069] (3) heating the solution in step (2) to 80° C. under stirring until the water is evaporated;

[0070] (4) the product in step (3) is put into a quartz boat after being ground, then placed in a tube furnace, under N 2 Under the atmosphere, the temperature was raised to 950°C at a heating rate of 5°C / min, kept for 60 minutes, and then lowered to room temperature at a cooling rate of 5°C / min to obtain carbon powder;

[0071] (5) The product obtained in step (4) was ground, washed by centrifugation with 1M HCl, washed with deionized water and absolute ethanol until neutral to remove impurities, and placed in a 60°C oven for vacuum drying. The resulting product is denoted as three-dimensional porous nitrogen-doped graphene-7.

[0072] The structural characterization of the three-dimensional po...

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Abstract

The invention provides a preparation method of three-dimensional porous nitrogen-doped graphene. The three-dimensional porous nitrogen-doped graphene is obtained by simultaneously using amino acid small molecules are a carbon source and a nitrogen source and sequentially performing roasting, grinding, pickling, washing with deionized water, washing with absolute ethyl alcohol and drying through a transition metal catalyst, the nitrogen source and a pore-forming activating agent are not needed to be added during the preparation process, the in-site porous nitrogen-doped graphene can be formed by an one-step method, and the three-dimensional porous nitrogen-doped graphene in different morphologies can be obtained according to different types of the transition metal catalyst. The method is simple and convenient, is low in cost and can be widely applied to the fields of a fuel cell, a lithium ion battery, a supercapacitor and the like, and mass production is facilitated.

Description

technical field [0001] The invention relates to the technical field of new carbon materials, in particular to a preparation method of three-dimensional porous nitrogen-doped graphene, three-dimensional porous nitrogen-doped graphene and applications thereof. Background technique [0002] Graphene is a two-dimensional material composed of a single layer of carbon atoms, which was accidentally discovered in 2004 by Professor Geim from the United Kingdom through mechanical exfoliation. Because of its excellent electrical conductivity, ultra-high mechanical strength, and huge specific surface area, graphene has caused a research boom since its discovery and has been widely used in many fields. Graphene has important applications in the cathode and anode of fuel cells. A large number of studies have shown that graphene can be directly used as a cathode oxygen reduction catalyst and exhibit high activity; in addition, graphene can also be used as an excellent catalyst carrier, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90H01M4/96H01M4/36H01M4/587H01G11/42
CPCH01G11/42H01M4/362H01M4/587H01M4/9091H01M4/96Y02E60/10Y02E60/13Y02E60/50
Inventor 孟辉杨世宏袁黎明
Owner 佛山市利元合创科技有限公司
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