Preparation method and application of nitrogen-doped graphene/nitrogen-doped carbon nanotube/zinc cobaltite composite material

A technology of nitrogen-doped graphene and nitrogen-doped carbon, which is applied in the field of electrochemistry, can solve the problems that are not involved in the research of supercapacitors, are not suitable for large-scale promotion and application, and fail to reduce the stacking of graphene, so as to achieve the improvement of composite materials. , not easy to overlap, shorten the effect of the distance

Active Publication Date: 2016-01-06
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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Problems solved by technology

[0004] In the existing graphene-supported zinc cobalt oxide technology, the stacking between graphene sheets is limited, so the overall volume utilization rate is low, such as Dr. Gao Guoxin, Professor Ding Shujiang, and Nanyang Technological University, Singapore. The synthesis method of graphene-loaded ultra-thin nickel cobaltate nanosheets researched by Professor XiongWen (David) Lou of the University ("Zinc Cobaltate Nanostructures Loaded on Graphene Surface") uses sodium citrate as the material, which was not used in the preparation process. It can reduce the stacking of graphene, and the materials studied are applied to lithium-ion batteries, and no further research has been done on supercapacitors; the

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  • Preparation method and application of nitrogen-doped graphene/nitrogen-doped carbon nanotube/zinc cobaltite composite material
  • Preparation method and application of nitrogen-doped graphene/nitrogen-doped carbon nanotube/zinc cobaltite composite material
  • Preparation method and application of nitrogen-doped graphene/nitrogen-doped carbon nanotube/zinc cobaltite composite material

Examples

Experimental program
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[0030] Example 1

[0031] (1) Disperse 3g of natural flake graphite in 70ml of 98% concentrated sulfuric acid, add 0.1g of sodium nitrate under ice bath to cool down, then add 9g of potassium permanganate, keep the temperature below 20℃, The reaction was stirred at a rate of 500 rpm for 1.5 hours; then the reactants were placed in a hot water bath at 38-40°C, and the reaction was stirred at a rate of 300-500 rpm for 30 minutes; then the reactants were taken out and placed in an ice-water bath again. Add distilled water and let stand for at least 2 hours. After the solution is stratified, discard the supernatant and centrifuge (13000rpm) for 10min, take the dark solution obtained by centrifugation, ultrasonic (20kHz) for 10min; then centrifuge again (4000rpm) for 10min, centrifuge The upper yellow transparent liquid obtained later is graphene oxide;

[0032] (2) Adjust the concentration of graphene oxide obtained in step (1) to 0.5 mg / ml, take 100 ml of graphene oxide into a beaker...

Example Embodiment

[0045] Example 2 Test of the influence of hydrothermal reaction temperature on composite materials

[0046] Taking Example 1 step (5) hydrothermal reaction temperature (120°C, 130°C, 140°C) as variables, the effects of different graphene and carbon nanotube ratios on the properties of composite materials were tested. The experiments were divided into the following groups:

[0047] Group 1: The mass ratio of porous graphene to carbon nanotubes is 5:1;

[0048] Group 2: The mass ratio of porous graphene to carbon nanotubes is 10:1;

[0049] Group 3: The mass ratio of porous graphene to carbon nanotubes is 15:1;

[0050] Group 4: No carbon nanotubes are added;

[0051] Group 5: Graphene does not make holes;

[0052] In Groups 1-4, except that the ratio of porous graphene to carbon nanotubes is added in step (3), and the hydrothermal reaction temperature in step (5) is different, the rest of the steps are the same as in Example 1;

[0053] Group 5 is the same as Example 1 except that it lacks ...

Example Embodiment

[0058] Example 3 Test of the influence of different calcination temperatures on the properties of composite materials

[0059] Taking the calcination reaction temperature (300°C, 350°C, 400°C) of step (6) in Example 1 as variables, the effect of different graphene and carbon nanotube ratios on the properties of composite materials was tested. The test is divided into:

[0060] Group 1: The mass ratio of porous graphene to carbon nanotubes is 5:1;

[0061] Group 2: The mass ratio of porous graphene to carbon nanotubes is 10:1;

[0062] Group 3: The mass ratio of porous graphene to carbon nanotubes is 15:1;

[0063] Group 4: No carbon nanotubes are added;

[0064] Group 5: Graphene does not make holes;

[0065] In Groups 1-4, except that the ratio of porous graphene to carbon nanotubes is added in step (3), and the calcination reaction temperature in step (6) is different, the rest of the steps are the same as in Example 1;

[0066] Group 5 is the same as in Example 1 except for the lack of ...

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Abstract

The invention discloses a preparation method of a nitrogen-doped graphene/nitrogen-doped carbon nanotube/zinc cobaltite composite material. The method comprises the following specific steps: (a) adding potassium permanganate, hydrochloric acid and hydrogen peroxide to graphene oxide, and carrying out a stirring reaction to obtain porous graphene; (b) dialyzing the porous graphene for 8-12 days, carrying out ultrasonic dispersion, then adding a carbon nanotube, carrying out ultrasonic mixing and carrying out suction filtration to form a film; (c) drying the film, and then adding ammonium hydroxide for reaction for 24 hours; (d) adding zinc nitrate, cobalt nitrate, urea, ammonium fluoride, absolute ethyl alcohol and distilled water for reaction for 4 hours; and (e) transferring a mixture to a tube furnace, and sintering the mixture in a nitrogen atmosphere for 2 hours, so as to obtain the composite material. The composite material has relatively good flexibility; the electrochemical properties are barely changed after the composite material is bent into various angles; the specific capacitance value of the composite material can be up to 1802F/g; compared with relatively simple graphene, the carbon nanotube and most of composite materials of the graphene and the carbon nanotube, the composite material provided in the invention are significantly improved.

Description

technical field [0001] The invention belongs to the field of electrochemistry, in particular to a preparation method and application of a nitrogen-doped graphene / nitrogen-doped carbon nanotube / zinc cobaltate composite material. Background technique [0002] Graphene is the thinnest and hardest known in the world nanomaterials , the thickness is only one carbon atom, and the specific surface area is as high as 2630m 2 / g, because the graphene-supported metal oxide or sulfide nanocomposite material can be used as the electrode material of electrochemical energy storage devices such as lithium-ion batteries, supercapacitors, and lithium-air batteries, which can significantly improve the charge / ion transport capacity of electrode materials , thereby improving the cycle stability of the electrode material. However, the reported metal oxides or sulfides supported on the surface of graphene mainly exist in the form of fine nanoparticles, with relatively low specific surface area,...

Claims

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Application Information

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IPC IPC(8): H01G11/36H01G11/86H01M4/90H01M4/88
CPCY02E60/50
Inventor 佟浩白文龙张校刚高珍珍岳世鸿幸四川
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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