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Preparation method of carbon nanometer tube-graphene composite material

A carbon nanotube and composite material technology, applied in the field of nanocomposite material preparation and application, can solve the problems of many graphene defects, limited growth, difficult interface contact, etc., to achieve simple process, strong interface contact, easy batch production effect

Active Publication Date: 2013-04-24
TSINGHUA UNIV
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Problems solved by technology

[0003] At present, the method of preparing composite materials that take into account the characteristics of carbon nanotubes and graphene basically adopts the method of physical mixing (Nano Lett.9, 1949-55, 2009), and the basic process is to combine the precursors of carbon nanotubes and graphene— Graphite oxide is simply mechanically mixed in the solution, and then the graphite oxide is reduced to become a hybrid composite material of carbon nanotubes and reduced graphene. However, in such composite materials, the relationship between carbon nanotubes and graphene only depends on physical bonding It is difficult to form a good interfacial contact, so the synergistic performance of carbon nanotubes and graphene is greatly reduced
Using the method of in-situ growth, the catalyst of carbon nanotubes can be loaded on the graphite oxide sheet for in-situ growth, and after further reduction, the composite material of carbon nanotubes-graphene can also be prepared (Adv.Mater.22, 3723-3728, 2010), however, there are many defects in the growth of carbon nanotubes on graphite oxide sheets, the growth is limited, and the preparation of related supported catalysts is also difficult to control, which also makes the prepared carbon nanotubes-graphene composites Limited performance and practical application space
In addition, by directly preparing a mixed catalyst of carbon nanotubes and graphene, and then using the method of in-situ growth, a composite material of carbon nanotubes-graphene can also be grown (application number: CN201210141649.6), but the method prepared The growth of carbon nanotubes is still limited, and there are many defects in graphene. In order to achieve real applications, the uniformity of materials and the control of process costs need to be strengthened.

Method used

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Embodiment 1

[0034] Ultrasonic dispersion of 5.0 g of magnesium hydroxide and 5.0 g of block copolymer P123 in 1 L of deionized water, and spray drying to obtain a magnesium oxide powder product with a particle size of ~1000 nm. The purified vermiculite array multi-walled carbon nanotubes were dispersed in the ionic liquid, and 50 g of a carbon nanotube suspension in which the mass percentage of the carbon nanotubes accounted for 0.6% in the solution was prepared. Add 1.0 g of magnesia powder catalyst to the above suspension, and stir evenly to form a mixture suspension of the two. The suspension of the above mixture is filtered and separated to form a powder product in which purified multi-walled carbon nanotubes and graphene catalyst particles are uniformly mixed. The mixed powder was put into 550° C. of nitrogen for calcination for 1 hour, then the temperature was raised to 900° C., and methane was introduced as a carbon source for vapor-phase chemical deposition for 20 minutes. The pr...

Embodiment 2

[0036]2.0 g of magnesium oxide particles were directly ultrasonically dispersed in 2 L of deionized water, filtered and dried to obtain magnesium oxide powder with a particle size distribution of 50-200 nm. Disperse the raw aggregated multi-walled carbon nanotube particles in ethanol, and prepare 50 g of agglomerated carbon nanotube particle suspension in which the mass percentage of carbon nanotubes accounts for 2.0% in the solution. Add 1.0 g of magnesium oxide powder to the above solution, and stir to form a mixture suspension. The suspension of the above mixture is filtered and separated to obtain a powder product in which the agglomerated carbon nanotubes and the magnesium oxide catalyst are uniformly mixed. This powder product is put into the nitrogen of 500 DEG C and calcined for 1 hour, then continues to heat up to 900 DEG C, feeds ethylene as carbon source and carries out gas-phase chemical deposition for 2 hours. Soak the obtained powder product in a hydrochloric ac...

Embodiment 3

[0038] 1.0 g of magnesium oxide particles and 5.0 g of block copolymer F127 were ultrasonically dispersed in 1 L of deionized water with a high-power ultrasonic rod, filtered and dried to obtain magnesium oxide nanoparticles with a particle size distribution of 10-100 nm. Disperse the purified single-walled carbon nanotubes in nitrogen methyl pyrrolidone, and prepare 50 g of a carbon nanotube suspension in which the mass percentage of uniformly dispersed carbon nanotubes accounts for 0.05% in the solution. Add 0.2 g of magnesium oxide particles to the above suspension, mix well to form a mixture suspension. The above mixture suspension was filtered to form a free-standing membrane. The film was calcined in argon at 600°C for 1 hour, then heated to 800°C, and passed through propyne for vapor phase chemical deposition for 5 minutes. The film product that obtains is soaked in the hydrochloric acid solution of mass percentage composition 14%, removes magnesium oxide catalyst part...

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Abstract

The invention discloses a preparation method of a carbon nanometer tube-graphene composite material, and the method comprises the following steps of: directly mixing uniformly dispersed carbon nanometer tubes and a catalyst for graphene uniformly, causing the graphene to grow in situ in a carbon nanometer tube network by means of chemical vapor deposition, and removing the catalyst for the graphene after purification treatment to obtain the carbon nanometer tube-graphene composite material. The carbon nanometer tube-graphene composite material gives consideration to the characteristics of both the carbon nanometer tube and the graphene, and has significant application values in the aspects such as electrochemical energy storage, catalyst preparation, a transparent electroconductive film, enhancement, electric conduction, and an adsorption material as well as a desorption material, and in addition the preparation method is simple in operation, low in cost and easy for industrial production and is an important preparation method of a nanometer carbon material.

Description

technical field [0001] The invention relates to a method for preparing a carbon nanotube-graphene composite material, which belongs to the field of preparation and application of nanocomposite materials. Background technique [0002] Carbon nanocomposites have a wide range of applications, especially in the fields of electrochemical energy storage, catalyst preparation, transparent conductive films, conductive materials, reinforcing materials, adsorption and desorption materials, etc. Among them, carbon nanotubes and graphene in carbon nanomaterials have extremely excellent characteristics. Carbon nanotubes have a high aspect ratio, good electrical conductivity and mechanical strength, while graphene has a large specific surface area, as well as excellent electrical conductivity and mechanical properties, and can combine the characteristics of these two carbon nanomaterials to design a more Ideal carbon nanocomposites have extremely important value and significance. [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B31/04C01B32/168C01B32/186
Inventor 魏飞贾希来
Owner TSINGHUA UNIV
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