Preparation method of heteroatom-doped graphene

A heterogeneous atom, graphene technology, applied in graphene, nano-carbon and other directions, can solve the problems of complex process, high cost, environmental pollution, etc., and achieve the effect of simplifying operation steps, reducing preparation cost, and enriching active sites.

Inactive Publication Date: 2019-05-21
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problems of environmental pollution, high cost and complicated process in the existing preparation method of hetero

Method used

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  • Preparation method of heteroatom-doped graphene
  • Preparation method of heteroatom-doped graphene
  • Preparation method of heteroatom-doped graphene

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Dissolve 10g of urea and 1g of citric acid in a mixed solution of 100mL of alcohol and 100mL of deionization, stir in a water bath at 85°C until it reaches a sol-gel state, and dry the resulting sol-gel in an oven at 100°C for 8 hours to obtain a precursor. The obtained precursor was loaded into a quartz boat, heated to 850° C. in a tube furnace for 5 h, and then lowered to room temperature to obtain nitrogen-doped graphene.

[0027] From scanning electron microscope photographs (see figure 1 a) It can be seen that the prepared nitrogen-doped graphene is in a uniform sheet shape.

[0028] figure 1 b is a transmission electron microscope photo of nitrogen-doped graphene. It can be seen that the color of each part of the graphene sheet is uniform, and it is tulle-like. figure 2 An atomic force microscope image of nitrogen-doped graphene. As can be seen from the figure, the height of nitrogen-doped graphene is about 3nm.

[0029] From the XRD figure of product (see ...

Embodiment 2

[0031] Dissolve 5 g of urea and 1 g of glucose in a mixed solution of 150 mL of alcohol and 100 mL of deionization, stir in a water bath at 85 °C until it reaches a sol-gel state, and dry the resulting sol-gel in an oven at 100 °C for 8 hours to obtain a precursor. The obtained precursor was loaded into a quartz boat, heated to 750°C in a tube furnace for 5 hours, and cooled to room temperature to obtain nitrogen-doped graphene. The nitrogen-doped graphene obtained has similar morphology to the nitrogen-doped graphene obtained in Example 1.

Embodiment 3

[0033] Dissolve 10g of urea, 1g of citric acid and 5g of thiourea in a mixed solution of 100mL of alcohol and 100mL of deionization, stir in a water bath at 85°C until it is in a sol-gel state, and dry the resulting sol-gel in an oven at 100°C for 8 hours to obtain a precursor . The obtained precursor was loaded into a quartz boat, heated to 1200 °C in a tube furnace for 2 h, and then lowered to room temperature to obtain nitrogen-sulfur co-doped graphene. The obtained nitrogen-sulfur co-doped graphene has a similar tulle-like morphology to the nitrogen-doped graphene in Example 1. Figure 4 The XRD spectrum and XPS general spectrum of nitrogen-sulfur co-doped graphene show the successful doping of S. By analysis, the atomic percentages of doped N and S are 20.52at% and 3.51at%, respectively.

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Abstract

The invention discloses a preparation method of heteroatom-doped graphene. The method comprises the steps of dissolving a nitrogen source and a carbon source into a solvent in a ratio, stirring in a water bath to obtain a sol gel, drying the sol gel to obtain a precursor and sintering the precursor at a high temperature to obtain nitrogen-doped graphene. Nitrogen sulfur, nitrogen boron or nitrogenphosphorus can be doped by adding a material containing other doping element such as thiourea, sulfuric acid, boric acid, ammonium borate, phosphoric acid or ammonium phosphate to the raw materials.Multi-element co-doped graphene is obtained by adjusting the ratio of the nitrogen source to the carbon source, controlling the pyrolysis temperature and time, and adding controllable doping content and type of other non-metal element compounds. The prepared doped graphene has high specific surface area, excellent electrical conductivity and rich active sites, and can be used as an electrode material in the field of electrochemical energy storage/ conversion.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and relates to a method for preparing graphene doped with heterogeneous atoms. Background technique [0002] Graphene is made of carbon atoms with sp 2 The monoatomic layer structure formed by hybridization has unique properties such as high stability, strong conductivity, and large theoretical specific surface area. Graphene composite electrode materials have high energy density and low internal resistance, which can realize high-rate charge and discharge. However, single-layer graphene is prone to re-stacking during the process of preparation and use, resulting in a decrease in its surface area and affecting the electrochemical performance of graphene. The doping of heteroatoms in the perfect hexagonal carbon of pure graphene can prevent the re-stacking of graphene, generate defects on the basal plane, generate energy band gaps, and accelerate the transport rate of charges, impro...

Claims

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Application Information

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IPC IPC(8): C01B32/184
Inventor 夏晖马依凡杨梅郭秋波徐璟翟腾
Owner NANJING UNIV OF SCI & TECH
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