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Method for preparing carbon nano tube with great inside diameter and controllable length

A carbon nanotube and large inner diameter technology, which is applied in the field of carbon nanotube preparation by catalytic chemical vapor deposition, can solve the problems of uneven tube diameter and uncontrollable length, and achieve the effect of simple equipment, more carbon source and solvent, and low cost

Inactive Publication Date: 2010-12-29
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, in the existing preparation technology, the diameter distribution of the prepared carbon nanotubes is below 50nm, and the pipe diameter is not uniform; and the length is uncontrollable

Method used

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  • Method for preparing carbon nano tube with great inside diameter and controllable length
  • Method for preparing carbon nano tube with great inside diameter and controllable length
  • Method for preparing carbon nano tube with great inside diameter and controllable length

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Experimental program
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Effect test

Embodiment 1

[0022] The synthesis is carried out in a horizontal quartz reactor. Under the condition of nitrogen protection, the temperature is raised to 950 ° C ~ 1100 ° C, the heating rate is 10 ~ 20 ° C / min, and the hydrogen gas is introduced at 10 ~ 100 L / h for about 5 minutes. Finally, the xylene solution in which ferrocene, sulfur, and thiophene are dissolved is input by the advection pump, and the catalyst solution is sprayed into the end of the reactor. The concentration is 50-80mg / ml, the thiophene concentration is 0.2-0.5ml / 100ml, the molar ratio of ferrocene to sulfur is 10:0.5-10:2, the nitrogen flow rate is 50-100L / h, and the reaction time is 60 minutes. The black flocculent product was collected at the end of the quartz tube and the exhaust gas bottle, and was determined to be 100-700nm carbon fibers by scanning electron microscope and transmission electron microscope, and there were amorphous carbon spheres at the same time. The yield was 4-6g, which was 15-20 times that ...

Embodiment 2

[0024] The synthesis reaction is carried out in a horizontal quartz reactor, and the temperature is raised to 950 ° C ~ 1100 ° C under the protection of nitrogen gas, the heating rate is 10 ~ 20 ° C / min, and hydrogen gas is fed 10 ~ 100 L / h. After about 5 minutes, The xylene ethanol solution dissolved with ferrocene, sulfur, and thiophene is input by a horizontal flow pump, the injection rate is 0.1-0.5ml / min, the volume ratio of ethanol to xylene is 1:1-2:1, and the concentration of ferrocene The concentration of thiophene is 0.2-0.5ml / 100ml, the ratio of ferrocene to sulfur is 10:0.5-10:2, the nitrogen flow rate is 80-100L / h, and the reaction time is 60 minutes. A black flocculent product was collected at the end of the quartz tube and the tail gas bottle, with a yield of 3-5 g, about 15-20 times that of the catalyst. As measured by scanning electron microscope and transmission electron microscope, the tube diameter is 40-70nm multi-walled carbon nanotubes, the inner dia...

Embodiment 3

[0026] The synthesis reaction is carried out in a horizontal quartz reactor, and the temperature is raised to 950 ° C ~ 1100 ° C under the protection of nitrogen gas, the heating rate is 10 ~ 20 ° C / min, and hydrogen gas is fed 10 ~ 100 L / h. After about 5 minutes, The xylene ethanol solution dissolved with ferrocene, nickelocene, sulfur and thiophene is introduced by a convection pump, the injection rate is 0.1-0.5ml / min, the concentration of ferrocene is 30-40mg / ml, ferrocene and The mass ratio of nickelocene is 10:0.02~10:0.05, the concentration of thiophene is 0.2~0.5ml / 100ml, the molar ratio of ferrocene to sulfur is 10:0.5~10:2, and the nitrogen flow rate is 80~100L / h , the reaction time is 60 minutes. A black flocculent product was collected at the end of the quartz tube and the tail gas bottle, with a yield of 3-5 g, about 15-20 times that of the catalyst. As measured by scanning electron microscope and transmission electron microscope, the tube diameter is 40-70nm...

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Abstract

The invention discloses a method for preparing a carbon nano tube with great inside diameter and controllable length. Mixed liquid of dimethyl benzene and ethanol is used as a carbon source, a mixture of dicyclopentadienyl iron and dicyclopentadienyl nickel is used as a catalyst, nitrogen or hydrogen is used as a carrier gas, a mixture of sulfur and thiophane is used as an additive, and the carbon nano tube with great inside diameter and controllable length is prepared in a horizontal electric furnace at 950 to 1,100 DEG C by adopting a floating catalysis method. A proper amount of dicyclopentadienyl nickel is added into the dicyclopentadienyl iron to form iron-nickel alloy nano granules so as to regulate the carbon settling speed of the catalyst, enlarge the inside diameter of the carbon tube and shorten the length of the carbon tube. The method has the advantages of convenient and simple operation, low cost, no pollution and simple equipment, and realizes low-cost batch preparation.

Description

technical field [0001] The invention belongs to the field of inorganic material synthesis and relates to the preparation of carbon nanotubes by catalytic chemical vapor deposition. Background technique [0002] Carbon nanotubes are tubular nano-scale graphite crystals, which are hollow tubular structures formed by curling single-layer or multi-layer graphite sheets around the central axis at a certain helical angle. Filling and loading specific materials in the inner cavity and outer surface of carbon nanotubes, combined with the oxidation resistance and thermal stability of carbon nanotubes, functional nanocomposites with specific uses can be obtained, such as filling iron, which can be used for magnetic recording, and loading iron oxide Body can be used for microwave absorption. Studies have shown that obtaining carbon nanotubes with a suitable hollow structure is the basis for their filling and loading. Studying the influence of controlling the hollow structure of multi...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 周固民瞿美臻
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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