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Method and device for mass growth of high-quality, straight carbon nanotubes in low-temperature gas phase

A carbon nanotube, high-quality technology, applied in the field of carbon nanotube preparation, can solve problems such as uneven diameter of carbon nanotubes, unstable catalyst supply, excess catalyst supply, etc., achieve good industrialization prospects, uniform diameter and reliable The effect of control and low usage

Active Publication Date: 2016-01-13
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] One of the purposes of the present invention is to provide a method for growing high-quality, straight carbon nanotubes in a low-temperature gas phase in a large amount and a special device thereof, which overcomes the problem of excess catalyst supply and the problem of oversupply of the current floating catalyst chemical vapor deposition method for growing carbon nanotubes. The catalytic efficiency of the catalyst is low, the catalyst precursor gradually agglomerates with the growth time, and the catalyst supply is unstable, so that the diameter of the obtained carbon nanotubes is not uniform, etc.

Method used

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  • Method and device for mass growth of high-quality, straight carbon nanotubes in low-temperature gas phase
  • Method and device for mass growth of high-quality, straight carbon nanotubes in low-temperature gas phase
  • Method and device for mass growth of high-quality, straight carbon nanotubes in low-temperature gas phase

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Effect test

Embodiment 1

[0039] device such as figure 1 As shown, catalyst precursor (ferrocene powder), growth promoter (sulfur powder), porous silica powder (average particle size is 100nm, average pore diameter is 7nm, porosity 35%) by weight ratio 100:1:1000 The ratio is mixed evenly and placed in the reaction device figure 1 in the programmed temperature heating pack. The flow rate in the reaction zone is 10ml / cm 2 Raise the temperature to 1000 °C under the protection of hydrogen for min, raise the temperature-controlled heating bag with the catalyst precursor to 40 °C, and feed the carbon source trichlorobenzene (8×10 -5 Gram equivalent carbon / min·cm 2 ) and carrier gas hydrogen (20ml / cm 2 min), increase the hydrogen flow directly into the reactor to 15ml / cm 2 min, carbon nanotubes start to grow, and the growth time is 20 min. In this embodiment, the supply amount of the catalyst precursor is 2×10 -8 Gram equivalent / hour·cm 2 , the supply of growth promoter is 2×10 -10 Gram equivalent / h...

Embodiment 2

[0042] device such as figure 1 As shown, catalyst precursor (ferrocene powder), growth promoter (sulfur powder), porous silica powder (average particle size is 10nm, average pore diameter is 2nm, porosity 50%) by weight ratio 100:1:1000 The ratio is mixed evenly and placed in the reaction device figure 1 in the programmed temperature heating pack. The flow rate in the reaction zone is 10ml / cm 2 Raise the temperature to 1000 °C under the protection of hydrogen for min, raise the temperature-controlled heating bag with the catalyst precursor to 30 °C, and feed the carbon source methane (1×10 -5 Gram equivalent carbon / min·cm 2 ) and the carrier gas hydrogen (5ml / cm 2 ·min), through the etchant water vapor (6×10 -6 Gram equivalent water / min·cm 2 , the free radicals are hydrogen and hydroxyl radicals), and the hydrogen flow directly into the reactor is increased to 15ml / cm 2 ·min, carbon nanotubes start to grow, and the growth time is 40min. In this embodiment, the supply a...

Embodiment 3

[0045] The device adopts a vertical reaction furnace, catalyst precursor (nickelocene powder), growth promoter (thiophene), porous magnesium oxide powder (average particle size 500nm, average pore diameter 80nm, porosity 80%) in a weight ratio of 100:1 : 1000% mixed evenly, placed in the reaction device figure 1 in the programmed temperature heating pack. The flow rate in the reaction zone is 10ml / cm 2 Under the protection of hydrogen for min, the temperature was raised to 600°C, and the programmed temperature control heating bag with the catalyst precursor was raised to 30°C, and the carbon source ethanol (2×10 -4 Gram equivalent carbon / min·cm 2 ) and the carrier gas hydrogen (5ml / cm 2 min), increase the hydrogen flow directly into the reactor to 15ml / cm 2 ·min, carbon nanotubes start to grow, and the growth time is 40min. In this embodiment, the supply amount of the catalyst precursor is 2×10 -8 Gram equivalent / hour·cm 2 , the supply of growth promoter is 2×10 -10 Gr...

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Abstract

The invention relates to a preparation technology of a carbon nanotube, and particularly discloses a method and a special device for low-temperature gas-phase macro growth of a high-quality straight carbon nanotube. A catalyst precursor, a growth promoter and inert agent powder are mixed evenly at normal temperature, and input into a reaction zone by a carrier gas and a carbon source at constant speed and low level; the reaction zone is a vertical or horizontal tube furnace; the growth temperature is 500-1000 DEG C; the catalyst precursor is an organic compound of Fe, Ni or Co, an inorganic salt, pure metal powder and the like, and the supply amount is 2*10<-8> to 2.9*10<-7> gram equivalent weight / hour.cm<2>; the growth promoter is a sulfur organic compound, and the supply amount is 1*10<-10> to 2.9*10<-9> gram equivalent weight / hour.cm<2>; the carbon source is a small molecule hydrocarbon, and the supply amount is 1*10<-5> to 3.9*10<-4> gram equivalent weight / minute.cm<2>; the carrier gas is argon or nitrogen or helium or hydrogen, and the supply amount is 1-100ml / minute.cm<2>. An etching agent needs to be introduced in the growth process, and macro production of the straight carbon nanotube with high purity, high quality and small diameter at low cost and low energy consumption is achieved.

Description

technical field [0001] The invention relates to the preparation technology of carbon nanotubes, in particular to a method for growing high-quality, straight carbon nanotubes in a low-temperature gas phase in a large quantity and a special device thereof. Background technique [0002] Carbon nanotubes have excellent mechanical properties, chirality-dependent conductive properties, ballistic transport properties, good flexibility and low density, etc., and are expected to be widely used in high-tech fields such as aviation, aerospace, and nanoelectronic devices . At present, the most common production method of carbon nanotubes is chemical vapor deposition. There are two main methods of chemical vapor deposition, namely substrate method and flow catalyst method. The preparation of commercially produced carbon nanotubes mainly adopts the substrate method, that is, the catalyst is impregnated / coated on a certain substrate, such as: porous zeolite, MgO, silicon substrate, etc., ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/02B82Y40/00C01B32/162C01B32/164
Inventor 侯鹏翔刘畅成会明石超丛洪涛
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI