Method for preparing metal filling carbon nano-pipe

A technology of metal filling and carbon nanotubes, applied in the direction of nanostructure manufacturing, nanotechnology, nanotechnology, etc., can solve the problems of high reaction temperature, low purity and yield, difficult product composition and structure, etc., and achieve a wide range of options , simple process, good controllability

Inactive Publication Date: 2009-02-18
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it is difficult to obtain high-purity target products by this method
In addition, metal-filled carbon nanotubes can also be obtained by directly pyrolyzing carbon-containing metal compounds at a certain temperature [Liu SW et al, preparation and characteristics of carbon nanotubes filled with cobalt, Chem.Mater.2000: 12(8) : 2205-11; Zhi LJ et al, Solid-state pyrolyses of metalphthalocyanines: a simple approach towards nitrogen-doped CNTs and metal / carbon nanocables, Small 2005: 1: 798-801], in comparison, this pyrolysis method The operation process is relatively simple, but the raw materials need to use expensive and toxic Co(CO)NO, Fe(Co)-phthalocyanine, etc., the purity and yield are very low, and the reaction temperature is also high
Therefore, so far, the yield of metal wire-filled carbon nanotubes obtained by the above preparation method is very low, and the control of product composition and structure is still a big problem.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018]Refined petroleum heavy oil by catalytic cracking (element content: C 90.48, H 8.80, C / H 0.86, N≤0.3) and analytically pure ferrocene are uniformly mixed in a mass ratio of 1:0.35, and placed in a high-pressure reactor middle. The reaction was heated under continuous mechanical stirring and nitrogen protection. The heating rate was maintained at 2.5°C / min. After reaching 450°C, the heating was stopped, and the temperature was naturally lowered to obtain pyrolysis products. The yield was 50wt%, and the self-increasing pressure of the system reached 5.4MPa. The reaction product was subjected to repeated thermal extraction (temperature 110° C.) with pyridine as a solvent until the filtrate became colorless and clear. The filter residue after drying is the metal-filled carbon nanotube with a yield of 70%. The elemental analysis results show that the mass percentage of metallic iron is about 14.0%, and the content of carbon element is 82.0%. Carry out X-ray diffraction (XRD...

Embodiment 2

[0020] The operation method is the same as in Example 1, the mass ratio of refined petroleum heavy oil to analytically pure ferrocene is 1:1, and the rest of the conditions remain unchanged. After co-pyrolysis and solvent extraction, Fe 3 Nano-iron rod / carbon composite material composed of C, with a diameter distribution of 15-30nm and a length distribution of 30-100nm. As confirmed by X-ray diffraction, the interlayer spacing (d 002 ) is 0.344nm, in order to further improve the degree of crystallization of carbon, the nano-iron rod / carbon composite material was oxidized at 250°C for 30 minutes and then carbonized at 1000°C, the d of carbon 002 The value decreases to 0.338nm, indicating that the orderly arrangement of carbon has been greatly improved.

Embodiment 3

[0022] The operation method is the same as in Example 1, the mass ratio of refined petroleum heavy oil to analytically pure ferrocene is 1:0.25, and the other conditions are unchanged. After carbonization and solvent extraction, it is mainly composed of α-Fe and Fe 3 A nano-iron rod / carbon composite material composed of C, with a diameter distribution of 40-50nm and a length distribution of 60-100nm.

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Abstract

The invention relates to a method for preparing a metal-stuffing carbon nanometer pipe; aromatic compound is adequately mixed with the transitional metal compound, and the mixture is undertaken the thermal condensation polymerization reaction and is extracted to get the metal-stuffed carbon nanometer pipe. The present invention has the advantages that the source of the raw materials is rich, the craftwork is simple, the preparation cost of the material is low, the purity is high, the selective range of the metal is wide, and the like, and the large-scale production is easy to be realized.

Description

Technical field: [0001] The invention relates to a method for preparing metal-filled carbon nanotubes. Background technique: [0002] Since Iijima discovered carbon nanotubes in 1991, filling fullerenes, metal nanoparticles and nanowires in carbon nanotubes, especially filling magnetic nanomaterials, has attracted great interest from researchers. Because carbon nanotubes can imprison metal substances in a small space, these filling materials have peculiar electrical, magnetic and optical properties. Okuyama F et al, Formation of carbon nanotubes and their filling with metallic fibers on ion-emitting field anodes, J.Appl.Phys.1998:84(3):1626-31] and absorbing materials [Che RC et al, Microwave absorption enhancement and complex permittivity and permeability of Fe encapsulated within carbon nanotubes, Adv. Mater. 2004: 16 (5): 401-5] and many other fields have potential applications. [0003] At present, the preparation methods of metal-filled carbon nanotubes are mainly div...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82B3/00
Inventor 宋怀河霍俊平陈晓红
Owner BEIJING UNIV OF CHEM TECH
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