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

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

CN105225844AActive Publication Date: 2016-01-06NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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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
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Disperse 3g of natural flake graphite in 70ml of concentrated sulfuric acid with a mass fraction of 98%, add 0.1g of sodium nitrate to cool down in an ice bath, then add 9g of potassium permanganate, keep the temperature below 20°C, and use 300- Stir the reaction at a rate of 500rpm for 1.5 hours; then place the reactant in a hot water bath at 38-40°C, and stir the reaction at a rate of 300-500rpm for 30min; Add distilled water and let it stand for at least 2 hours. After the solution is layered, discard the supernatant and centrifuge (13000rpm) for 10min. Take the dark solution obtained by centrifugation and ultrasonicate (20kHz) for 10min; then centrifuge again (4000rpm) for 10min. The upper yellow transparent liquid obtained afterward 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 in a beaker, add 1.5 g of potassium permanganate, stir and react at a rate of 300-500 rpm fo...

Embodiment 2

[0045] Embodiment 2 hydrothermal reaction temperature influence test on composite material

[0046] Taking the hydrothermal reaction temperature (120°C, 130°C, 140°C) in step (5) of Example 1 as a variable, the influence of different ratios of graphene and carbon nanotubes on the performance of composite materials was tested. The tests 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: without adding carbon nanotubes;

[0051] Group 5: Graphene does not create 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 that of...

Embodiment 3

[0058] Example 3 Different calcination temperatures affect the performance of composite materials

[0059] Taking the calcination reaction temperature (300°C, 350°C, 400°C) in step (6) of Example 1 as a variable, the influence of different ratios of graphene and carbon nanotubes on the performance of composite materials was tested. The tests were 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: without adding carbon nanotubes;

[0064] Group 5: Graphene does not create 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 that of Example 1 excep...

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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

Patent Timeline
06 Jan 2016
Publication
CN105225844A
IPC
H01G11/36; H01G11/86; H01M4/90; H01M4/88
CPC
Y02E60/50
Inventors
佟浩; 白文龙