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Method for preparing spiral nano carbon fiber

A carbon nanofiber and helical technology, which is applied in the field of preparing helical carbon nanofibers, can solve the problems of difficult preparation of small-diameter catalysts, difficult to clean up, complicated preparation process, etc., and is conducive to mass production, the method is simple and easy to operate, and the wide The effect of the application foreground

Inactive Publication Date: 2007-07-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there are two kinds of reports at home and abroad about the preparation of spiral carbon fibers: chemical vapor deposition and pitch melt spinning. The preparation of spiral nano-carbon fibers generally adopts chemical vapor deposition (CVD), with low-carbon hydrocarbon compounds as carbon sources. Nano-Fe, Cr, Ni, Cu and their nano-alloy particles are used as catalysts to prepare spiral nano-carbon fibers. The preparation process of the above-mentioned nano-catalysts is very complicated, and the particle size is difficult to control. Generally, Fe, Cr, Ni, Cu and other metals The salt solution is adsorbed on the surface of ultra-fine silica and other particles, and then prepared by hydrogen reduction to prepare nano-metal catalysts attached to the surface of ultra-fine silica and other particles. These ultra-fine silica particles will be mixed in the helical nano-carbon fiber , it is difficult to clean
It is generally believed that the inner diameter of carbon fibers and carbon nanotubes is equal to the diameter of catalyst particles. People always try to obtain catalysts with smaller particle sizes, but the preparation of small diameter catalysts is difficult and expensive, and its application is limited to a certain extent.

Method used

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  • Method for preparing spiral nano carbon fiber
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Experimental program
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Effect test

Embodiment 1

[0015] Before the reaction, the nickel plate catalyst with a thickness of 1mm and a length and width of 150mm and 30mm was subjected to surface treatment, and the surface of the nickel plate was subjected to high-speed sandblasting for 30 minutes, then soaked in dilute hydrochloric acid for 5 hours, dried and placed in a tube furnace In the constant temperature zone, the nickel plate catalyst is placed horizontally on the graphite plate; the reaction system is evacuated, replaced with nitrogen three times, and nitrogen is introduced. The flow rate of nitrogen is 200ml / min. Simultaneously add PCl with hydrogen as carrier gas 3 Cocatalyst, PCl 3 The flow rate of cocatalyst is 0.03ml / min, the ratio of diluent gas nitrogen and acetylene flow is 2.5:1 (wherein: acetylene is 40ml / min, nitrogen is 100ml / min), the ratio of hydrogen and acetylene flow is 3:1 (wherein : Acetylene is 40ml / min, hydrogen is 120ml / min), and the reaction constant temperature time is 35min, carries out catal...

Embodiment 2

[0017] Before the reaction, the nickel plate catalyst with a thickness of 1.5mm and a length and width of 150mm and 30mm was subjected to surface treatment, and the surface of the nickel plate was subjected to high-speed sandblasting for 30 minutes, then soaked in dilute sulfuric acid for 8 hours, dried and placed in a tubular In the constant temperature zone of the furnace, the nickel plate catalyst is vertically placed on a horizontal graphite plate; the reaction system is evacuated, replaced with argon for three times, and fed with argon. The flow rate of argon is 200ml / min, and the temperature is raised to At 670°C, add PCl with hydrogen as the carrier gas while feeding acetylene 3 Cocatalyst, PCl 3 The flow rate of co-catalyst is 0.04ml / min, the ratio of diluent gas argon to acetylene flow is 2:1 (among them: acetylene is 50ml / min, argon is 100ml / min), the ratio of hydrogen to acetylene flow is 3.5:1 (Among them: acetylene is 50ml / min, hydrogen is 175ml / min), the reactio...

Embodiment 3

[0019] Before the reaction, the nickel plate catalyst with a thickness of 0.5mm and a length and width of 150mm and 30mm was subjected to surface treatment, and the surface of the nickel plate was subjected to high-speed sandblasting for 30 minutes, then soaked in dilute hydrochloric acid for 5 hours, dried and placed in a tubular In the constant temperature zone of the furnace, the nickel plate catalyst is placed horizontally on the graphite plate; the reaction system is evacuated, replaced with nitrogen three times, and nitrogen is introduced. The flow rate of nitrogen is 200ml / min, and the temperature is raised to 680°C under nitrogen atmosphere, and acetylene is introduced. While adding PCl with hydrogen as carrier gas 3 Cocatalyst, PCl 3 The flow rate of cocatalyst is 0.05ml / min, the ratio of diluent gas nitrogen and acetylene flow is 3:1 (wherein: acetylene is 45ml / min, nitrogen is 135ml / min), the ratio of hydrogen and acetylene flow is 4:1 (wherein : acetylene is 45ml / ...

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Abstract

The invention relates to a spiral nanometer carbon fiber, in detail the manufacturing method of spiral nanometer carbon fiber. In the invention the acetylene is carbon source, the hydrogen is carrier gas, the nitrogen or argon gas is diluent air, the nickel plate is catalyst, the PCl3 is cocatalyst. The spiral nanometer carbon fiber is produced by CVD in lower temperature. The invention is provided with simple method and process, easy control, low cost, high output and purity, and convenience industrial production. Prepared spiral nanometer carbon fiber is provided with wide application prospect in strengthening structure, absorbing material and microelectronic device so on.

Description

technical field [0001] The invention relates to a helical nano-carbon fiber, in particular to a method for preparing a helical nano-carbon fiber. Background technique [0002] Spiral carbon fiber is a functional carbon fiber, which can be obtained by solid-phase carbonization of high-molecular organic fibers or gas-phase catalytic pyrolysis growth of low-molecular hydrocarbons. It has the heat resistance, chemical stability, electrical and thermal conductivity of general carbon fibers, It has excellent properties such as low thermal expansion, friction resistance, low wear, low density, and good biocompatibility, and its special helical shape endows the material with typical chiral characteristics, good elasticity, and good combination with the matrix. As a new type of electromagnetic wave absorber, micro-sensitive energy absorber, stealth material, micro-mechanical components such as micro-springs, etc., it has broad application prospects in the fields of structural reinfor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/127
Inventor 赵东林沈曾民于建民
Owner BEIJING UNIV OF CHEM TECH
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