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A kind of preparation method and application of three-dimensional porous heteroatom-doped graphene

A three-dimensional porous, heteroatom technology, used in chemical instruments and methods, catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, etc., can solve problems such as insufficient utilization of specific surface area, and achieve good development. The effect of foreground, reducing agglomeration and increasing specific surface area

Inactive Publication Date: 2017-01-25
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the strong van der Waals force between graphene sheets, it is easy to aggregate and stack during the preparation process, resulting in the inability to fully utilize its huge specific surface area.

Method used

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  • A kind of preparation method and application of three-dimensional porous heteroatom-doped graphene
  • A kind of preparation method and application of three-dimensional porous heteroatom-doped graphene
  • A kind of preparation method and application of three-dimensional porous heteroatom-doped graphene

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Embodiment 1

[0027] The invention provides a method for preparing three-dimensional porous heteroatom-doped graphene, the three-dimensional porous heteroatom-doped graphene is prepared by a hard template method, and the steps are as follows:

[0028] In the first step, 200mg graphene oxide, 700mg dicyandiamide, 200mgFeCl 2 4H 2 O and 500mg of silicon dioxide with a diameter of 7nm were uniformly dispersed in ethanol by ultrasonic, heated and stirred at 60°C for 24h, and dried at 85°C to obtain the precursor. The above mass content is based on the total mass of the precursor.

[0029] Wherein, the mass percentage of graphene oxide is 12.5 wt%, the mass percentage of nitrogen atom precursor is 43.75 wt%, the mass percentage of non-noble metal salt is 12.5 wt%, and the mass percentage of template agent is 43.75 wt%.

[0030] In the second step, the above precursor is placed in a quartz boat, and under the protection of nitrogen, the temperature is raised to 900°C at 5°C / min for calcination ...

Embodiment 2

[0042] A preparation method of three-dimensional porous heteroatom-doped graphene is as follows:

[0043] In the first step, 1350mg graphene oxide, 75mg boric acid, 15mgFeSO 4 7H 2 O and 60mg of silicon dioxide with a diameter of 30nm were uniformly dispersed in water by ultrasonic, heated and stirred at 60°C for 24h, and dried at 85°C to obtain the precursor.

[0044]Wherein, the mass percent of graphene oxide is 90wt%, the mass percent of nitrogen atom precursor is 5wt%, the mass percent of non-noble metal salt is 1wt%, and the mass percent of templating agent is 4wt%. The above mass content is based on the total mass of the precursor.

[0045] In the second step, the above-mentioned precursor is placed in a quartz boat, and under the protection of nitrogen, the temperature is raised to 600°C at 10°C / min for calcination and reduction treatment for 1 hour, and a solid product is obtained after cooling.

[0046] The third step is to treat the solid product with a blend of h...

Embodiment 3

[0048] A preparation method of three-dimensional porous heteroatom-doped graphene is as follows:

[0049] The first step, 1050mg graphene oxide, 270mg diphenyl disulfide, 30mgFe(C 2 h 3 o 2 ) 2 and 150 mg of silicon dioxide with a diameter of 300 nm were uniformly dispersed in chloroform by ultrasonic, heated and stirred at 60° C. for 24 hours, and dried at 85° C. to obtain a precursor.

[0050] Wherein, the mass percent of graphene oxide is 70wt%, the mass percent of nitrogen atom precursor is 18wt%, the mass percent of non-noble metal salt is 2wt%, and the mass percent of templating agent is 10wt%. The above mass content is based on the total mass of the precursor.

[0051] In the second step, the above precursor is placed in a quartz boat, and under the protection of argon, the temperature is raised to 800°C at 15°C / min for calcination and reduction treatment for 2h, and a solid product is obtained after cooling.

[0052] The third step is to treat the solid product wi...

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Abstract

The invention provides a preparation method of three-dimensional porous heteroatom-doped graphene. The preparation method comprises the following steps: (1) uniformly dispersing graphene oxide, a heteroatom precursor, a non-noble metal salt and a template agent into a solvent, thereby obtaining a precursor after heating, stirring and drying; (2) performing high-temperature roasting treatment on the precursor in the presence of inert gases, thereby obtaining solid products; and (3) treating the solid products by a blended solution of hydrofluoric acid and hydrochloric acid, removing the template and metals by one step, and then, re-heating to obtain the three-dimensional porous heteroatom-doped graphene. The invention further provides a method adopting the three-dimensional porous heteroatom-doped graphene to prepare a membrane electrode combined body. The three-dimensional porous heteroatom-doped graphene disclosed by the invention has a high specific surface area, and has a good application prospect in the fields such as fuel batteries, metal-air batteries as well as supercapacitors.

Description

technical field [0001] The invention belongs to the field of graphene materials, in particular to a preparation method and application of three-dimensional porous heteroatom-doped graphene. Background technique [0002] With the advent of the energy crisis and the increasingly serious environmental pollution, the development of sustainable energy storage and conversion technologies (such as fuel cells, metal-air batteries, supercapacitors, etc.) has attracted widespread attention. Among them, the oxygen reduction catalyst is an important component of these advanced technologies, which directly determines the performance and cost of these devices. At present, platinum or platinum alloys are the most effective oxygen reduction catalysts widely used. However, platinum is expensive and its reserves are limited, making the research on non-precious metal oxygen reduction catalysts a hot spot in the industry. [0003] Heteroatom-doped carbon materials have attracted extensive att...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J37/16B01J27/24B01J23/745B01J21/18B01J27/02B01J27/185
Inventor 乔锦丽周学俊张霞李雪梅李浩然刘予宇张久俊
Owner DONGHUA UNIV
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