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Method for direct and continuous preparing supershort carbon nanometer tube

A technology of carbon nanotubes and ultra-short carbon, applied in the field of nanometers, can solve the problems of continuous production with short discrete distribution, different lengths of carbon nanotubes, unfavorable large batches, etc., and achieve low gas prices, wide process range, and simple methods Effect

Inactive Publication Date: 2006-07-12
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The carbon nanotubes obtained by this method have different lengths, the steps are more complicated, the treatment time is long, and a lot of amorphous carbon will be produced during the oxidation process, which requires further treatment such as air oxidation.
[0003] After searching the literature of the prior art, it was found that Zhang Aifei and others from Beijing Institute of Technology [(ethanol-catalyzed cracking method to prepare a large number of discrete carbon nanotubes) "Fine Chemical Industry" 22 (2005), 658-660] had used ethanol as a carbon source to prepare Although this method solves the problem of directly preparing discrete carbon nanotubes, it uses dangerous or expensive gases such as hydrogen and helium as protective gases, and catalysts and carbon sources need to be processed during the reaction. Preheating, the obtained product is a mixture of single-wall and multi-wall tubes, and the product is deposited at the outlet of the reaction vessel, which is not conducive to large-scale, low-cost, continuous production of discretely distributed carbon nanotubes with short lengths
Therefore, so far, there is still no ideal method for the direct and continuous synthesis of ultrashort carbon nanotubes.

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The synthesis is carried out in a horizontal quartz tube reactor. Under the protection of argon, the temperature is raised to 1100°C, and the heating rate is 20°C / min, and then the ethanol dissolved in ferrocene and thiophene is fed by an electronic peristaltic pump. Solution, the concentration of ferrocene is 2g / 100ml, the concentration of thiophene is 3%, the feeding rate is 20ml / h, the flow rate of regulating argon is 160l / h, and the reaction time lasts 3 hours. A large amount of product can be collected in the collector. The collected product was dissolved in 1:1 HNO 3 The solution was refluxed at 110°C for 2 hours, then washed and dried with deionized water to obtain a purified product. The product is a multi-walled carbon nanotube with a diameter of about 15-20nm and a length of 100-300nm.

Embodiment 2

[0022] Under the protection of nitrogen, the temperature was raised to 1200°C at a rate of 20°C / min, and then the methanol solution dissolved with ferrocene and thiophene was passed through with an electronic peristaltic pump. The catalyst concentration was 1g / 100ml, and the thiophene concentration was 5%. The feed rate was 30ml / h, the nitrogen flow rate was adjusted to be 80l / h, and the reaction duration was 3 hours. A large amount of product can be collected in the collector. The collected product was dissolved in 1:1 HNO 3 The solution was refluxed at 110°C for 2 hours, then washed and dried with deionized water to obtain a purified product. The product is a multi-walled carbon nanotube with a diameter of about 15-30nm and a length of 200-400nm.

Embodiment 3

[0024] Under the protection of argon, the temperature was raised to 1000°C at a rate of 20°C / min, and then an acetone solution dissolved with carbonyl iron and thiophene was passed through an electronic peristaltic pump. The catalyst concentration was 3g / 100ml, and the thiophene concentration was 10%. The feed rate was 100ml / h, the nitrogen flow rate was adjusted to be 120l / h, and the reaction duration was 3 hours. A large amount of product can be collected in the collector. The collected product was dissolved in 1:1 HNO 3 The solution was refluxed at 110°C for 2 hours, then washed and dried with deionized water to obtain a purified product. The product is a multi-walled carbon nanotube with a diameter of about 15-20nm and a length of 100-400nm.

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Abstract

The invention discloses a making method of direct and continual ultrashort carbon nanometer pipe in the nanometer material technique domain, which comprises the following steps: adapting transition metal organics as catalyst and alcohol as carbon source and solvent; taking single-phase sulphur or organic compound as growth accelerant and inert gas as protection gas and carrier gas to anchor the carbon source and catalyst in the high temperature region rapidly; birdnesting the metal atom into nanometer metal particle in the high temperature region; decomposing the alcohol into carbon nanometer pipe under the high temperature and catalyzing action of transition metal particle; generating the carbon nanometer pipe to collect in the collector directly due to supplying alcohol and metal organics continually. The invention improves the obtaining rate and the product is easy to dispose, which is fit for commercialization produce and batch manufacturing.

Description

technical field [0001] The invention relates to a method in the field of nanotechnology, in particular to a method for directly and continuously preparing ultra-short carbon nanotubes. Background technique [0002] Carbon nanotubes have extremely wide application prospects due to their unique structure and excellent performance. However, for the application of carbon nanotubes, fields such as hydrogen storage and catalyst supports require a large number of short-length, open-end, and discretely distributed carbon nanotubes, but the carbon nanotubes prepared by a large number of preparation methods are agglomerated The length together reaches several microns, which is very unfavorable to the application. In order to obtain short carbon nanotubes required for application, the following two methods are commonly used at present: ball milling method and oxidation method. The ball milling method is to use ball milling equipment to physically destroy carbon nanotubes to achieve t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 王健农苏连锋牛钧杰
Owner SHANGHAI JIAO TONG UNIV
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