Floating catalyst chemical vapor deposition method of single-walled carbon nanotubes

A single-walled carbon nanotube, chemical vapor deposition technology, applied in the direction of single-walled carbon nanotubes, carbon nanotubes, chemical instruments and methods, etc., can solve the problems of low growth efficiency and carbon source conversion rate, and improve the carbon source The effect of conversion rate, increased yield, and reduced impurity content

Active Publication Date: 2019-03-08
唯碳纳米科技(沈阳)有限公司
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Problems solved by technology

[0005] At present, the floating catalyst chemical vapor deposition process can already prepare high-quality single-walled carbon nanotubes (document 4: Song Jiang, Peng-Xiang Hou, Mao-Lin Chen, Bing-Wei Wang, Dong-Ming Sun, Dai- Ming Tang, Qun Jin, Qing-Xun Guo, Ding-Dong Zhang, Jin-Hong Du, Kai-Ping Tai, Jun Tan, Esko I. Kauppinen, Chang Liu, Hui-Ming Cheng. Ultrahigh-performance transparent conductive films of carbon- welded isolated single-wall carbon nanotubes Science Advances.2018; 4:eaap9264), but its growth efficiency and carbon source conversion rate are very low, and the carbon source conversion rate is generally lower than 5%

Method used

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  • Floating catalyst chemical vapor deposition method of single-walled carbon nanotubes

Examples

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Effect test

Embodiment 1

[0032]In this example, a mixed solution of toluene, ferrocene, and thiophene (hereinafter referred to as the mixed solution) with a mass ratio of 100:7.5:1.5 was prepared first, and was subjected to ultrasonic treatment for 10 minutes for later use. Under the protection of a hydrogen atmosphere, the temperature of the horizontal tube furnace was raised to 1200°C, then the hydrogen flow rate was adjusted to 4300sccm, and 11sccm ethylene was introduced, and 2ppm water vapor was introduced at the same time, and then the prepared mixed solution was fed with 0.9ml / h It is injected into the horizontal tube furnace at a constant speed, and enters the reaction zone under the carrying of the mixed gas of hydrogen and ethylene to grow carbon nanotubes. The reaction time is 1 hour.

[0033] Such as figure 1 Shown, the optical picture of obtained product, this sample weight is 350mg. Using the yield calculation formula: η=(sample weight / gram equivalent of carbon source used)×100%, the ca...

Embodiment 2

[0036] In this example, firstly, a mixed solution of toluene, ferrocene and thiophene with a mass ratio of 100:6:1.6 was prepared, and the solution was ultrasonically treated for 10 minutes for later use. Under the protection of a hydrogen atmosphere, raise the temperature of the horizontal tube furnace to 1100°C, then adjust the hydrogen flow rate to 3900sccm, and feed 11sccm ethylene and 0.5ppm water vapor at the same time, then feed the prepared mixed solution at 0.9ml / h The rate is injected into the horizontal tube furnace at a constant speed, and enters the reaction zone under the carrying of the mixed gas of hydrogen and ethylene to grow carbon nanotubes. The reaction time is 1.5 hours. Under the process parameters, the carbon source conversion efficiency is 17%, the obtained sample has high purity, the catalyst content is 1.08wt%, the crystallinity of carbon nanotubes is high, and the concentrated oxidation temperature is 785°C.

Embodiment 3

[0038] In this example, firstly, a mixed solution of toluene, nickelocene and thiophene with a mass ratio of 100:6:1.8 was prepared, and the solution was ultrasonically treated for 10 minutes for later use. Under the protection of a hydrogen atmosphere, the temperature of the horizontal tube furnace was raised to 1300°C, and then the hydrogen flow rate was adjusted to 4800 sccm, and 13 sccm of ethylene was introduced, and 3.5 ppm of water vapor was introduced at the same time, and then the prepared mixed solution was fed at a rate of 1 ml / h. It is injected into the horizontal tube furnace at a constant speed, and enters the reaction zone under the carrying of the mixed gas of hydrogen and ethylene to grow carbon nanotubes. The reaction time is 1.5 hours. Under the process parameters, the carbon source conversion efficiency is 22%, the obtained sample has high purity, the catalyst content is 1.02wt%, the crystallinity of carbon nanotubes is high, and the concentrated oxidation t...

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Abstract

The invention relates to the technical field of control preparation of carbon nanotubes, in particular to a floating catalyst chemical vapor deposition method of single-walled carbon nanotubes. Hydrogen is used as carrier gas, transition metal is used as a catalyst, sulfur is used as a growth promoter, trace vapor is introduced in a reaction system, the catalytic efficiency of the metal particle catalyst in a growth area is improved, the service life of the catalyst is prolonged, and efficient growth of the single-walled carbon nanotubes with high purity and high crystallinity degree is realized. The conversion efficiency of a carbon source is as high as 25% under an optimized condition; the prepared carbon nanotubes have uniform diameter, high crystallinity degree and the highest centralized oxidation-resistant temperature up to 816 DEG C; very few catalyst impurities are left and the content of the catalyst is lower than 1.1wt%. The method realizes high efficiency of the preparationprocess and high quality of products, provides an effective way for mass preparation and industrial development of high-quality single-walled carbon nanotubes, and has great significance in large-scale application of the high-quality single-walled carbon nanotubes.

Description

technical field [0001] The invention relates to the technical field of controlled preparation of carbon nanotubes, in particular to a floating catalyst chemical vapor deposition method for growing high-purity and high-crystallinity single-walled carbon nanotubes at a high conversion rate. Background technique [0002] Single-walled carbon nanotubes can be regarded as a seamless hollow tubular structure formed by curling a single layer of graphene along a certain direction. The uniqueness of this structure makes single-walled carbon nanotubes have excellent mechanical properties, chirality-dependent conductive properties, ballistic transport properties, excellent flexibility and high chemical stability, etc., and are expected to be used in aviation, aerospace, nanoelectronics Devices and other high-tech fields have been widely used. However, to realize the application of single-walled carbon nanotubes in the above fields, the first bottleneck problem that needs to be solved ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/162C01B32/159B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B32/159C01B32/162C01B2202/36C01B2202/30C01B2202/04C01B2202/02
Inventor 刘畅石超侯鹏翔成会明
Owner 唯碳纳米科技(沈阳)有限公司
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