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Large-area high-quality nitrogen-doped graphene as well as preparation method and application thereof

A nitrogen-doped graphene, large-area technology, applied in the field of graphene, can solve problems such as unfavorable C-N bonds, and achieve the effect of simple process, good structural quality, and high photoelectric performance

Inactive Publication Date: 2014-10-22
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Graphene with high nitrogen doping degree is usually difficult to obtain, because the higher the reaction temperature is, the more favorable it is for the formation of C-C bonds, and it is not conducive to the formation of C-N bonds.

Method used

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  • Large-area high-quality nitrogen-doped graphene as well as preparation method and application thereof
  • Large-area high-quality nitrogen-doped graphene as well as preparation method and application thereof
  • Large-area high-quality nitrogen-doped graphene as well as preparation method and application thereof

Examples

Experimental program
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preparation example Construction

[0043] The general preparation process is as follows:

[0044] The first step, the preparation of catalyst:

[0045] If copper foil, copper block, copper alloy, etc. are used, it can be used directly; if copper plating is used as a catalyst, copper can be evaporated on the substrate by electron beam evaporation and other methods; if a copper-containing compound is used as a catalyst, the compound can be dissolved In a certain solvent, it is attached to the substrate by spin coating or direct drop method, and it is used after being dried.

[0046] The second step: Spin-coat P4VP (polytetravinylpyridine) on the copper catalyst used as a carbon and nitrogen source and dry it in an oven

[0047] The third step: the reaction device such as figure 1 As shown, the copper catalyst with P4VP is placed in the low-temperature zone of the clean quartz tube, and then the air in the quartz tube is removed by repeated vacuuming three times, or 10-3000 sccm non-oxidizing gas (such as hydrog...

Embodiment 1

[0051] Example 1. Preparation of nitrogen-doped graphene with a high-quality crystal structure on a copper-based substrate

[0052] The first step: ultrasonically clean the copper foil with deionized water, ethanol, and acetone in sequence, then dry it in an oven, then spin-coat P4VP (polytetravinylpyridine, molecular weight 60,000) on its surface as a carbon and nitrogen source, and then dry it in an oven Internal drying, the average thickness of the film after drying is 100nm. The specific coating process is as follows: Take 40 μL of P4VP solution with a molar concentration of 0.1 mg / mL dissolved in chloroform solvent, and spin-coat evenly on a surface with a size of 1 cm. 2 ×1cm 2 copper foil surface. Place the P4VP-coated and dried copper foil in the low-temperature area of ​​a clean quartz tube, and then completely remove the air in the furnace by repeated vacuuming. Through 150sccm H 2 And 30sccm Ar mixed gas as carrier gas, start heating.

[0053] Step 2: When the ...

Embodiment 2

[0056] Embodiment 2, prepare nitrogen-doped graphene on copper-based substrate

[0057] The preparation method is basically the same as in Example 1, except that: when the temperature in the central area of ​​the furnace reaches 600° C., an iron bar is used to push the copper foil to the high temperature area. The Raman spectrum of the product is as Figure 7 As shown, it is proved that the product is graphene with 5-10 layer structure, and the nitrogen content is 8%.

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Abstract

The invention discloses a preparation method of large-area high-quality nitrogen-doped graphene. The nitrogen-doped graphene is prepared by taking a nitrogen-containing polymer as a precursor. The method comprises the following steps: coating a carbon and nitrogen source on the surface of a copper catalyst or putting on the copper catalyst, and then reacting under the condition of 600 DEG C to 900 DEG C in a non-oxidizing atmosphere so as to obtain the nitrogen-doped graphene, wherein the copper catalyst can be of elemental copper, a copper alloy or a copper-containing compound. The prepared nitrogen-doped graphene is of 1 to 10 layers of large-area films with high-quality crystal structures, and has the electrical characteristics of N-field effects and the light transmittance no matter under air or vacuum environment. The method provided by the invention is simple in process, economical, low in cost, simple and convenient to operate and suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of graphene, and in particular relates to a large-area high-quality nitrogen-doped graphene and a preparation method and application thereof. Background technique [0002] Graphene has many excellent properties due to its quasi-two-dimensional crystal structure, which has aroused great interest of researchers today. The electrical properties of ideal single-layer graphene have a linear relationship with the wave vector near the highest point of the hexagonal Brillouin zone, and have a weak quantum Hall effect and a bipolar electric field effect along the ballistic transmission at room temperature. It is precisely because of these unique properties of graphene that it has good application prospects in the fields of microelectronic devices, organic optoelectronic materials, energy storage materials, composite materials, biomedical materials, etc. Therefore, large-scale preparation of graphene with high-quality crystal s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 王朝晖闫寿科何冰
Owner INST OF CHEM CHINESE ACAD OF SCI
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