Nitrogen-doped carbon nano-tube array and graphene hybrid and preparation method thereof

A carbon nanotube array and graphene technology, which is applied in the field of carbon nanotube array and graphene hybrids and their preparation, can solve the problems of poor quality and morphology of carbon nanotubes, hindering electron transport, affecting performance expression, etc. Achieve the effect of easy engineering scale-up and large-scale preparation, and simple process

Active Publication Date: 2013-11-27
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the method of preparing similar hybrids is to directly support metal active components on the surface of graphite oxide to catalyze the growth of carbon nanotubes (Fan ZJ, et al., Adv. Mater. 2010, 22, 3723–3728), but due to the The particle is unstable on the graphite surface at high temperature, and the quality and morphology of the carbon nanotubes in the resulting product are poor, which affects the performance expression; or an intermediate oxide film is supported on the surface of the expanded graphite to assist the dispersion of the catalyst particles (Du F, et al. al., Chem. Mater.,2011, 23(21): 4810-4816), although the morphology of the product is good, but there is an oxide film layer between the carbon nanotube array and graphene that hinders electron transport

Method used

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  • Nitrogen-doped carbon nano-tube array and graphene hybrid and preparation method thereof

Examples

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Embodiment 1

[0032] Example 1: Using FeMo / white vermiculite as a catalyst to prepare a nitrogen-doped carbon nanotube array and graphene hybrid through a fixed bed.

[0033] Vermiculite is a common lamellar stacked material, which has good cleavage properties at high temperatures, a large radius of curvature, and a microscopic flat surface. White vermiculite was used as the catalyst carrier, and the catalyst whose active components Fe and Mo accounted for 20% and 2% of the total mass were obtained by impregnation and loading. The catalyst was placed in the center of a tubular fixed bed with an inner diameter of 20 mm, and the temperature was raised to 650 °C in an atmosphere of 200 sccm argon and 100 sccm hydrogen oC, followed by a mixture of carbon source ethylene and nitrogen source ammonia, the carbon-nitrogen atomic ratio is 1:1, the carbon source partial pressure is 25%, and the temperature is maintained for 30 min to grow nitrogen-doped carbon nanotube arrays by chemical vapor deposi...

Embodiment 2

[0034] Example 2: Using FeMoMg LDH as a catalyst to prepare a nitrogen-doped carbon nanotube array and graphene hybrid through a fixed bed.

[0035] LDH is a layered dihydroxy compound metal hydroxide with a hydrotalcite-like sheet structure and a large radius of curvature. Using FeMoMgLDH with active components of 30% and 3% of Mo content and 30% Mg content as the catalyst, it was placed in a fixed bed with an inner diameter of 20 mm, under the atmosphere of 200 sccm nitrogen and 50 sccm hydrogen Warm up to 700 o C, and then pass into the carbon source propylene, the carbon source partial pressure is 50%, and the temperature is maintained for 30 minutes to grow carbon nanotube arrays by chemical vapor deposition, then the carbon source and hydrogen are turned off, and the temperature is raised to 900 °C under a nitrogen atmosphere. o C, then feed the mixture of carbon source benzene and toluene and nitrogen source pyridine, the carbon-nitrogen atomic ratio is 1:5, the carbo...

Embodiment 3

[0036] Example 3: NiMo / vermiculite was used as a catalyst to prepare a nitrogen-doped carbon nanotube array and a graphene hybrid through a fixed bed.

[0037] Using vermiculite with Ni and Mo loadings of 1% and 0.1% as catalysts, it was placed in the center of a tubular fixed bed with an inner diameter of 50 mm, and the temperature was raised to 700 °C in an atmosphere of 200 sccm helium. o C, followed by a mixture of carbon source butene and nitrogen source pyridine, the carbon-nitrogen atomic ratio is 1:2, the carbon source partial pressure is 25%, and the temperature is maintained for 30 min to grow nitrogen-doped carbon nanotube arrays by chemical vapor deposition , then turn off the carbon source and nitrogen source, and raise the temperature to 1000 under the helium atmosphere o C, then feed a mixture of carbon source methane and nitrogen source ethylenediamine, the carbon-nitrogen atomic ratio is 1:1, the carbon source partial pressure is 30%, and react for 1 hr to gro...

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Abstract

The present invention discloses a nitrogen-doped carbon nano-tube array and graphene hybrid and a preparation method, and belongs to the technical field of carbon material preparation. The hybrid comprises a nitrogen-doped carbon nano-tube array and graphene, wherein the end portion of the carbon nano-tube array is directly and effectively connected with the graphene sheets. The preparation method comprises: adopting a high density catalyst particle loaded material having a microscopic flat surface as a catalyst, and adopting chemical vapor deposition to grow a nitrogen-doped carbon nano-tube array and graphene on the surface of the catalyst, wherein the nitrogen-doped carbon nano-tube array and the graphene are directly and effectively connected to form a three-dimensional structure. With the present invention, types of multifunction specialty nanometer carbon materials are enriched, assembly of nanometer carbon materials from bottom to top and from low-dimension to three-dimension is achieved, and a moving bed, a fluidized bed and the like can be adopted to achieve engineering magnification and scalization production so as to easily promote researches, supplies and practical applications of the nitrogen-doped carbon nano-tube array and graphene hybrid.

Description

technical field [0001] The invention belongs to the technical field of carbon material preparation, in particular to a hybrid of carbon nanotubes and graphene and a preparation method thereof, in particular to a hybrid of nitrogen-doped carbon nanotube arrays and graphene and a preparation method thereof. Background technique [0002] The progress and development of human society and the continuous improvement of daily life conditions are inseparable from the rapid changes of modern science and technology, and one of the most important parts is the development and preparation of new multifunctional materials. Since Iijima first successfully observed the clear structure of carbon nanotubes with high-resolution transmission electron microscopy in 1991 (Iijima S. Nature, 1991, 354(6348): 56-58), in 2004 Geim et al. used mechanical exfoliation to obtain single-layer graphene Since the structure (Novoselov K S et al., Science, 2004, 306(5696): 666-669), the family of carbon nanom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/00C01B31/02C01B31/04B82Y30/00C01B32/162C01B32/186
Inventor 魏飞唐城赵梦强张强黄佳琦
Owner TSINGHUA UNIV
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