Catalyst for growing three-dimensional carbon nanotube/grapheme composite material and preparation method of catalyst

A carbon nanotube and composite material technology is applied in the field of preparation of catalysts for the growth of three-dimensional carbon nanotube/graphene composite materials, and can solve problems such as unfavorable effective specific surface area and energy storage density, inability to fully and effectively exert characteristics, and inability to react. Go ahead and other problems to avoid uncontrollable temperature, easy control and realization, and prevent agglomeration

Active Publication Date: 2012-11-21
四川天策聚材科技有限公司
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  • Description
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  • Application Information

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Problems solved by technology

Chinese patent CN201110261623 discloses a method for preparing a graphene-carbon nanotube composite thin film based on a three-dimensional network morphology. characteristics of the
Chinese patent CN200910218482 discloses an in-situ preparation method of a graphene / carbon nanotube composite film, using a chemical vapor deposition (CVD) method to synthesize a graphene / carbon nanotube composite film in one step, and the prepared composite film is composed of Graphene sheets and carbon nanotubes overlap each other, but the carbon tubes are still intertwined, which is not conducive to the improvement of effective specific surface area and energy storage density.
Using the microwave heating method reported in the literature (microwave frequency: 2450MHz, power: 700W, heating time: 15min), the preparation of Ni / graphene oxide catalyst was carried out, and it was found that the reaction liquid appeared rapidly within 5 minutes during the heating precipitation process. Knocking, resulting in the inability of the reaction to proceed; the prepared catalyst is used for the growth of carbon nanotubes and is inactive

Method used

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  • Catalyst for growing three-dimensional carbon nanotube/grapheme composite material and preparation method of catalyst
  • Catalyst for growing three-dimensional carbon nanotube/grapheme composite material and preparation method of catalyst
  • Catalyst for growing three-dimensional carbon nanotube/grapheme composite material and preparation method of catalyst

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preparation example Construction

[0038] The specific steps of the catalyst preparation method for the growth of the three-dimensional carbon nanotube / graphene composite material of the present invention are:

[0039] 1) Dissolve the surfactant in deionized water, then add the graphene oxide suspension to the above solution, and disperse under ultrasonic conditions for 20-60 minutes to fully mix the surfactant and graphene oxide;

[0040] Wherein, the mass ratio of surfactant to nickel nitrate is 1-4, preferably 1.25; the surfactant is one of sodium lauryl sulfate and mercaptoacetic acid;

[0041] 2) Gradually add the nickel nitrate solution into the solution obtained in step 1) under vigorous stirring; wherein, the dropping rate of the nickel nitrate solution is 0.3-2ml / min (10mg / ml); the stirring speed is 250-325r / min; The mass ratio of nickel and graphene oxide is 0.5-6, preferably 4;

[0042] 3) Add urea to the solution obtained in step 2), and heat the mixed solution to 85-95°C (after heating urea in wat...

Embodiment 1

[0048] Assemble a 500mL reaction bottle in an ice-water bath, add 120ml of concentrated sulfuric acid, add a solid mixture of 5g of graphite powder and 2.5g of sodium nitrate under stirring, stir in an ice-water bath for 30min, then add 15g of potassium permanganate in portions to control the reaction The temperature does not exceed 20°C, stir and react for a period of time, then raise the temperature to about 35°C, continue to stir for 30 minutes, then slowly add a certain amount of deionized water, the temperature rises to 98°C, after stirring for 20 minutes, further dilute with water, and add 50ml of hydrogen peroxide (30%) to reduce the residual oxidant, so that the solution turns bright yellow; filter while hot, and wash with 5% HCl solution and deionized water until no sulfate group is detected in the filtrate; finally put the filter cake in a 60°C Fully dry in a vacuum drying oven; then 200mg graphene oxide is ultrasonically dispersed in 300ml deionized water for 40min t...

Embodiment 2-14

[0050] Compared with Example 1, only the catalyst component content, or the type of surfactant used, or the nickel nitrate solution drop rate, or the stirring speed are different, and the other processes are the same as in Example 1, and each finished catalyst is obtained. The catalyst composition of embodiment 2 to embodiment 14 and its used dropping speed and stirring speed are shown in table 1.

[0051] Table 1 Catalyst Composition Table

[0052]

[0053] Place the catalyst obtained in Examples 1-11 in the middle of the heating zone of the horizontal reaction furnace, raise the temperature to a reaction temperature of 850°C at a rate of 10°C / min under a nitrogen atmosphere, switch to methane (volume flow rate 100mL / min), react for 5 minutes, and close methane, and cooled to room temperature in a nitrogen atmosphere to prepare a three-dimensional carbon nanotube / graphene composite material sample.

[0054] The scanning electron micrograph of the three-dimensional carbon ...

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Abstract

The invention belongs to the technical field of new nano materials and particularly relates to a catalyst for growing a three-dimensional carbon nanotube / grapheme composite material and a preparation method of the catalyst. The catalyst is formed by taking urea as a precipitator and uniformly precipitating nitrate as an active component on a graphene oxide carrier of which the surface is adsorbed with a surfactant. The method is simple and controllable; the activity of the catalyst is high; and the prepared three-dimensional carbon nanotube / grapheme composite material is regular in morphology.

Description

technical field [0001] The invention belongs to the technical field of new nanometer materials, in particular to a method for preparing a catalyst for growing a three-dimensional carbon nanotube / graphene composite material. Background technique [0002] Carbon nanotubes and graphene are two typical carbon nanomaterials. Graphene is composed of single layer sp 2 A honeycomb-like two-dimensional planar crystal structure composed of hybridized carbon atoms; and a carbon nanotube is a one-dimensional cylindrical structure formed by curling graphene. Both can be used as electrode materials. Carbon nanotubes are considered as good candidates for high-power electrode materials due to their good electrical conductivity and easily accessible surface to the electrolyte. However, its specific surface area (generally 500m 2 g -1 ) is relatively small, and the energy density as an electrode material is low, which needs to be further improved. Although graphene has high electrical c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J37/00B01J37/03H01G9/042
Inventor 文婕李云涛
Owner 四川天策聚材科技有限公司
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