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Method of symmetrically growing spiral carbon tube

A technology of carbon tubes and spirals, applied in the field of symmetrical growth of nano-helical carbon tubes and their preparation, can solve problems such as complex conditions and difficult control, and achieve the effects of simple preparation process, narrow particle size distribution, and unique catalytic activity

Inactive Publication Date: 2007-04-18
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the current preparation mainly relies on doping impurities such as sulfur in the catalyst and introducing impure gas, the conditions are extremely complicated and difficult to control

Method used

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  • Method of symmetrically growing spiral carbon tube
  • Method of symmetrically growing spiral carbon tube
  • Method of symmetrically growing spiral carbon tube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: under strong stirring, 0.03mol FeCl 2 4H 2 O and 0.045mol citric acid were dissolved in 100mL of absolute ethanol, and stirred continuously at 60°C for 6 hours to form a uniform transparent sol; evaporated and dried at 80°C until a xerogel was formed; the xerogel was pre-baked at 450°C in air for 3 hours, and then An appropriate amount of this oxide is placed in a tube furnace and placed in a hydrogen atmosphere in the tube furnace for reduction at 450° C. for 4 hours. Then turn off the hydrogen, immediately introduce acetylene gas, keep warm at 450°C for 6 hours, and then cool to room temperature. The obtained carbon tube electron microscope observation results are shown in Figure 1, the field emission scanning electron microscope observation results are shown in Figure 2 and the XRD results are shown in Figure 3. The same molar amount of oxalic acid is also acceptable. Acetylene was maintained at 150 Pa in the growth chamber. The growth is highly symmetr...

Embodiment 2

[0023] Example 2: under strong stirring, 0.03mol FeCl 2 4H 2 O and 0.045mol citric acid were dissolved in 100mL of absolute ethanol, and stirred continuously at 60°C for 6 hours to form a uniform transparent sol; evaporated and dried at 80°C until a xerogel was formed; the xerogel was pre-baked at 450°C in air for 3 hours, and then Take an appropriate amount of this oxide and place it in a tube furnace in a hydrogen atmosphere at 450°C for 4 hours for reduction. Then turn off the hydrogen, immediately introduce acetylene, keep warm at 450°C for 6 hours, then cool to room temperature, and then quickly heat up to 750°C, then turn off the acetylene, immediately introduce argon, keep at 750°C for 4 hours, and then cool to room temperature. The obtained XRD results are shown in FIG. 4 .

Embodiment 3

[0024] Example 3: The experimental process and conditions are the same as in Example 1, but the amount of catalyst is 3 times that of Example 1. The obtained carbon tube scanning electron microscope observation results are shown in Figure 5. It is also possible to reduce the temperature at 600 ° C for 3 hours, and the acetylene is maintained at 100 Pa.

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Abstract

The present invention relates to a method for symmetrically growing spiral carbon tube. Said method includes the following steps: using ferrous chloride of ferrous sulfate as raw material, using citric acid as complexing agent and using absolute alcohol as solvent, making the above-mentioned materials undergo the process of complexation reaction to obtain sol, evaporating and drying said sol to form gel, precalcining said gel at 80-120 deg.C in air to remove organics to form dry gel, then sintering said dry gel at 450 deg.C to obtain oxide nano iron powder body, using said powder body as catalyst precursor and placing it into a ceramic magnetic boat, and placing it into a quartz tube, making reduction reaction at 450 deg.C in H2 atmosphere so as to obtain nano iron catalyst; the mode ratio of ferrous chloride or ferrous sulfate and citric acid is 1:1.0-1:5.0, complexation reaction temperature is 50-90 deg.C, precalcining temperature of dry gel in the air is 300-600 deg.C, its reduction temperature is 300-900 deg.C, reduction time is 3-6 h; closing hydrogen gas, promptly introducing acetylene gas, and heat-insulating for 5-7 h.

Description

1. Technical field [0001] The invention relates to a highly symmetrical symmetrical growth nano-helical carbon tube nanometer and a preparation method thereof. In particular, iron catalyst nanoparticles and methods for their preparation. 2. Background technology [0002] In the preparation method of CN200410065511.8 chiral helical carbon fiber, the inventor of the present invention grows highly symmetrically with iron nanoparticles as the center, and the particle diameter of the carbon fiber is about the diameter of the iron particle. The preparation method takes iron oxide as the catalyst precursor, and the oxide uses ferrous chloride or ferrous sulfate as the raw material, citric acid as the complexing agent, and absolute ethanol as the solvent to form a uniform non-aqueous sol. It is obtained by drying in air to form xerogel after complexation, and pre-baking in air to remove organic matter. Reduction at 450°C in H2 atmosphere can obtain Fe nanoparticle catalyst. Howev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B81B3/00B01J23/745
Inventor 汤怒江都有为
Owner NANJING UNIV