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Method for repairing graphite structure in reduced graphene oxide and application of nitrogen-doped reduced graphene oxide

A technology of graphite structure and graphene, applied in the application of nitrogen-doped reduced graphene oxide, repairing the field of graphite structure in reduced graphene oxide, can solve the problem of affecting the physical and chemical properties of graphene, low specific capacitance, and destroying the integrity of graphite structure In order to achieve the effects of large-scale production, mild conditions and excellent electrochemical performance

Pending Publication Date: 2020-02-14
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Due to its excellent physical and chemical properties, graphene is widely used in the fields of electronic devices, optoelectronic devices, energy storage, biomaterials and probes; and the methods of preparing graphene mainly include chemical vapor deposition, mechanical or liquid phase exfoliation , reduced graphene oxide method, etc.; compared with chemical vapor deposition and mechanical or liquid phase exfoliation, graphene prepared by reduced graphene oxide method has advantages such as simple operation, no need for overly complicated instruments and equipment, and mild conditions. Good application prospects; but because a large number of oxygen-containing functional groups and many defects are introduced, the physical and chemical properties of the prepared graphene are affected; for example: the thermal conductivity, electron mobility, and mechanical properties of reduced graphene oxide are far away lower than that of graphene prepared by mechanical exfoliation; in recent years, reduced graphene oxide has been widely used as an electrode material for supercapacitors, but its specific capacitance is far lower than its theoretical specific capacitance; by introducing nitrogen atoms into reduced graphene oxide , can greatly improve the specific capacitance of reduced graphene oxide; but the amorphous carbon formed by the nitrogen-containing substance introduced will destroy the integrity of the graphite structure; in the existing technology, through different small molecules (such as pyridine, Benzene, etc.) as precursors on base catalysts (copper, platinum, palladium, etc.) conditions; therefore, it is still a challenge to introduce nitrogen atoms into graphene at lower temperatures and form graphitic nitrogen-doped carbon

Method used

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  • Method for repairing graphite structure in reduced graphene oxide and application of nitrogen-doped reduced graphene oxide
  • Method for repairing graphite structure in reduced graphene oxide and application of nitrogen-doped reduced graphene oxide
  • Method for repairing graphite structure in reduced graphene oxide and application of nitrogen-doped reduced graphene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Under stirring conditions, 6 mL of pyridine was added to the suspension of 3.5 mL of graphene oxide, and then 33.3 mg of nickel sulfate hexahydrate was dissolved in 10.5 mL of deionized water and added to the above solution; the mixed solution was sealed in poly Then the container was kept at 180°C for 6 hours; the polytetrafluoroethylene container was cooled to room temperature and the solution was freeze-dried, and the resulting solid was calcined at 300°C for 1 hour at a heating rate of 5°C / min. Hour. After cooling down to room temperature, wash with 300mL 1M hydrochloric acid and 1000mL deionized water, and dry; carry out XPS spectrogram analysis on the sample that has not been washed with 1M hydrochloric acid after calcination, and the figure 2 As can be seen, it can be seen that it contains a trace amount of nickel elemental substance through its nickel peak, and these trace amounts of nickel elemental substance can catalyze pyridine to form nitrogen-doped graphi...

Embodiment 2

[0032] The application of the nitrogen-doped reduced graphene oxide prepared on supercapacitor electrode materials comprises the following steps under optimal conditions:

[0033] Carbon black, polytetrafluoroethylene suspension and the prepared nitrogen-doped reduced graphene oxide are mixed in a mass ratio of 1:1:8 to form a slurry, and then the coating is coated on a stainless steel current collector (1cm -2 ), and then pressed at a pressure of 20 MPa for 10 minutes to make it closely contact with the current collector, and then vacuum-dried at 80°C for 24 hours. Obtain the electrode material that can be applied on the supercapacitor; In the three-electrode system, the silver / silver chloride electrode is used as the reference electrode, the platinum electrode is used as the counter electrode, and the electrolyte is 6M potassium hydroxide; in the two-electrode system, the The prepared two electrode materials and the cellulose separator were assembled into a "sandwich" type; ...

Embodiment 3

[0041] Embodiments 1 and 2 are the best preferred schemes of the present invention, and the following Table 1 and Table 2 are the single factor optimization experiments carried out in the process of obtaining the best preferred schemes of Example 1 in obtaining Examples 1 and 2. Except that the conditions considered to be investigated are different from those in Example 1, other conditions are the same as in Examples 1 and 2.

[0042] Capacitance data table under different current densities of materials prepared by the technology of the present invention under different pyridine ratios in table 1

[0043] Current density (A / g) 1 2 5 10 20 GOPD 300 Ni 1.7 (F / g)

416.2 347.6 315.0 293.0 264.0 GOPD 250 Ni 1.7 (F / g)

368.1 308.2 272.5 245.0 224.0 GOPD 350 Ni 1.7 (F / g)

384.6 315.4 286.5 263.0 234.0

[0044] Capacitance data table of the material prepared by the technology described in the present invention under diffe...

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Abstract

The invention belongs to the field of preparation of graphene oxide, and particularly relates to a method for repairing a graphite structure in reduced graphene oxide, wherein the method comprises thefollowing steps: (1) oxidizing graphite to prepare graphene oxide; and (2) mixing the graphene oxide prepared in the step (1) with pyridine to prepare a mixed solution, adding a predetermined amountof nickel ions into a mixed solution, carrying out a hydrothermal reaction on the mixed solution, carrying out freeze drying on the product after the reaction is completed, calcining at a predetermined temperature for a predetermined time, and washing and drying the calcined solid to obtain the target product. Compared with a vapor deposition method, the implementation conditions of the technologyfor repairing the graphite structure in the reduced graphene oxide and introducing a nitrogen-containing functional group do not need specific complex equipment and harsh conditions; the preparationmethod is simple to operate, low in cost, mild in condition and beneficial to large-scale production; and meanwhile, the prepared nitrogen-doped reduced graphene oxide has excellent electrochemical performance.

Description

technical field [0001] The invention belongs to the field of preparation of graphene oxide, and in particular relates to a method for repairing graphite structure in reduced graphene oxide and the application of nitrogen-doped reduced graphene oxide. Background technique [0002] Due to its excellent physical and chemical properties, graphene is widely used in the fields of electronic devices, optoelectronic devices, energy storage, biomaterials and probes; and the methods of preparing graphene mainly include chemical vapor deposition, mechanical or liquid phase exfoliation , reduced graphene oxide method, etc.; compared with chemical vapor deposition and mechanical or liquid phase exfoliation, graphene prepared by reduced graphene oxide method has advantages such as simple operation, no need for overly complicated instruments and equipment, and mild conditions. Good application prospects; but because a large number of oxygen-containing functional groups and many defects are...

Claims

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Application Information

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IPC IPC(8): C01B32/184H01G11/32
CPCC01B32/184H01G11/32C01B2204/22Y02E60/13
Inventor 钟文斌陈泽宇谭兮亦
Owner HUNAN UNIV
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