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New method for preparing nitrogen doped graphene

A technology of nitrogen-doped graphene and organic ligands, which is applied in the field of graphene, can solve the problems of nitrogen content and distribution position uncertainty, and achieve the effects of convenient operation, simple preparation process and high electrochemical performance

Active Publication Date: 2013-06-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the above traditional methods of preparing nitrogen-doped graphene, the doped nitrogen is often distributed in the defects of the material, and the nitrogen content and distribution position are uncertain.

Method used

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  • New method for preparing nitrogen doped graphene
  • New method for preparing nitrogen doped graphene
  • New method for preparing nitrogen doped graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] The first step: Add 4.908mmol of bis(1,5-cyclooctadiene) nickel and 4.908mmol of 2,2′‐bipyridine into a round bottom flask, then add 78ml of purified DMF, and then add 4.908mmol of 1,5-Cyclooctadiene, stir the mixture until completely dissolved. 0.942 mmol of organic ligand TBT was added to the purple solution obtained above. React at 95°C for 8 hours. After the solution was cooled to room temperature, 29.9 ml of concentrated hydrochloric acid was added to the dark purple solution, and the color of the solution became light green and transparent. The solution was filtered and washed with 5×19.5 ml of chloroform, 5×19.5 ml of tetrahydrofuran and 5×19.5 ml of deionized water, respectively. Transfer to a vacuum oven and dry at 200°C for 7 hours to obtain COP-4 solid powder.

[0049] Step 2: Put the covalent organic polymer COP-4 with a mass of 0.05g in a tube furnace. Before heating up the tube furnace, vacuumize it first, and then pass in an inert gas. Then rise from ...

Embodiment 2

[0054] The preparation method and experimental conditions are basically the same as in Example 1, except that the organic ligand used is TBP, that is, the carbonized material is C-COP-P. Such as Figure 5 Shown are the Raman spectra and scanning electron micrographs of the products. From the scanning electron microscope image, it can be seen that the material is a mixture of spherical particles and rod-like structures, but it can be seen that the rod-like structures are curled from layered structures. The positions and intensities of the peaks in the Raman spectrum are consistent with the structure of nitrogen-doped graphene.

Embodiment 3

[0056] The preparation method and experimental conditions are basically the same as in Example 1, except that the organic ligand used is TBTT, that is, the carbonized material is C-COP-T. Such as Figure 6 Shown is a scanning electron micrograph of the product. It can be seen from the figure that the prepared material has a uniform structure and mainly exists in a layered structure.

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Abstract

A method for preparing nitrogen doped graphene belongs to the technical field of graphene. An appropriate organic compound is selected and a covalent organic polymer material is prepared through nickel-catalytic Yamamoto coupled reaction; in a programmed heating tubular furnace, the material is used as a carbon source and also a template, and carbonized at a high temperature to prepare a high-performance nitrogen-doped graphene powder material. The method is simple in preparation process, convenient for operation, easy to implement and free of extra nitrogen source; and the content and the distribution of the nitrogen element can be accurately controlled by screening the matrix.

Description

technical field [0001] The invention relates to a new method for preparing nitrogen-doped graphene by high-temperature carbonization of covalent organic polymers, and belongs to the technical field of graphene. Background technique [0002] Graphene is a carbon atom with sp 2 A new type of material with a monolayer sheet structure composed of hybrid orbitals. In 2004, Andre Geim and Konstantin Novoselov, physicists at the University of Manchester, UK, successfully separated graphene from graphite in experiments, thus confirming that graphene can exist alone. Graphene is a new type of material with high electrical and thermal conductivity, high specific surface area, high mechanical strength and toughness. In addition, graphene is able to maintain high mobility at high doping levels. These properties make graphene widely used as an electrode component and electrocatalyst in the field of energy storage and conversion. [0003] The electrical and chemical properties of grap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04B82Y30/00C01B32/184
Inventor 曹达鹏张鹏向中华
Owner BEIJING UNIV OF CHEM TECH
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