Macro and controllable preparation method of large-diameter and narrow-diameter distribution single-walled carbon nano-tubes

A technology of single-walled carbon nanotubes and diameter distribution, applied in the direction of carbon nanotubes, nanocarbons, chemical instruments and methods, etc., can solve the problems of poor product uniformity, low proportion of single-walled carbon nanotubes, etc., and achieve low impurity content , Low amount of catalyst residue and complete structure

Active Publication Date: 2019-10-22
唯碳纳米科技(沈阳)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In comparison, the single-walled carbon nanotubes prepared by the floating catalyst chemical vapor deposition method have a larger diameter, but when the diameter is greater than 2.2nm, the number of carbon nanotube walls inevitably increases, and the resulting products are carbon nanotubes with different wall numbers. The mixture of tubes, the product uniformity is poor, and the proportion of single-walled carbon nanotubes is not high

Method used

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  • Macro and controllable preparation method of large-diameter and narrow-diameter distribution single-walled carbon nano-tubes
  • Macro and controllable preparation method of large-diameter and narrow-diameter distribution single-walled carbon nano-tubes
  • Macro and controllable preparation method of large-diameter and narrow-diameter distribution single-walled carbon nano-tubes

Examples

Experimental program
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Effect test

Embodiment 1

[0034] In this example, firstly, a mixed solution of toluene, ferrocene, and thiophene with a mass ratio of 100:9.5:2.5 was prepared, and ultrasonically treated for 10 minutes for later use. Under the protection of a small flow rate of 200 sccm hydrogen, raise the temperature of the chemical vapor deposition horizontal tube furnace to 1200 ° C, then adjust the hydrogen flow rate to 4300 sccm, and feed 10.5 sccm methane and 6.2 sccm ethylene at a rate of 0.53 ml / h A mixed solution prepared by toluene, ferrocene and thiophene was injected at a constant speed to grow carbon nanotubes for 1 hour. The sample was collected and weighed, the sample weighed 0.3g, and the carbon source conversion rate was calculated to be 25%.

[0035] Such as figure 1 As shown, the product sample is characterized by scanning electron microscope and transmission electron microscope. It can be seen from the typical scanning electron microscope photo of the prepared single-walled carbon nanotube that the...

Embodiment 2

[0037] In this example, firstly, a mixed solution of toluene, ferrocene and thiophene with a mass ratio of 100:10.3:2.6 was prepared, and ultrasonically treated for 10 minutes for later use. Under the protection of a small flow rate of 200sccm hydrogen, the chemical vapor deposition horizontal tube furnace was heated to 1200°C, then the hydrogen flow rate was adjusted to 4000sccm, and 17sccm methane and 6.9sccm ethylene were introduced at a constant rate of 0.54ml / h A mixed solution prepared by injecting toluene, ferrocene, and thiophene was injected to grow carbon nanotubes for 2 hours. The sample was collected and weighed, the sample weighed 0.21 g, and the carbon source conversion rate was calculated to be 17%.

[0038] The structure of the prepared carbon nanotubes was characterized by scanning electron microscope, transmission electron microscope and differential thermal analysis respectively. The large-diameter single-walled carbon nanotubes produced by this process par...

Embodiment 3

[0040] In this example, a mixed solution of toluene, ferrocene, and thiophene with a mass ratio of 100:7.8:2.0 was first prepared, and the solution was ultrasonically treated for 10 minutes for later use. Under the protection of a small flow rate of 200 sccm hydrogen, raise the temperature of the chemical vapor deposition horizontal tube furnace to 1200 °C, then adjust the hydrogen flow rate to 3800 sccm, and feed 13.5 sccm methane and 6.2 sccm ethylene at a rate of 0.53 ml / h A mixed solution prepared by toluene, ferrocene and thiophene was injected at a constant speed to grow carbon nanotubes for 1 hour. The sample was collected and weighed, the sample weighed 0.24g, and the carbon source conversion rate was calculated to be 20%.

[0041] The structure of the prepared carbon nanotubes was characterized by scanning electron microscope, transmission electron microscope and differential thermal analysis respectively. The large-diameter single-walled carbon nanotubes produced by...

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Abstract

The invention relates to the field of structural control preparation of single-walled carbon nano-tubes, particularly to a macro and controllable preparation method of large-diameter and narrow-diameter distribution single-walled carbon nano-tubes. According to the present invention, the macro preparation of large-diameter single-walled carbon nano-tubes is achieved by using a floating catalyst chemical vapor deposition method, such that the macro and controllable preparation of the single-walled carbon nano-tubes with diameters of greater than 2 nm and narrow diameter distribution is achieved, wherein the diameters of more than 95% of the carbon nano-tubes are distributed within 2.1-2.7 nm, the diameters of more than 87% of the carbon nano-tubes are distributed within 2.1-2.5 nm, the single-walled carbon nano-tubes have characteristics of high purity and less impurities, the residual amount of the catalyst is less than 4.1 wt%, he single-walled carbon nano-tubes have high crystallinity, and the highest anti-oxidation temperature is 809 DEG C; the single-walled carbon nano-tube fibers spun by a liquid phase method have high electrical conductivity, provide the material basis for the research on the nanometer confinement effect of single-walled carbon nano-tubes and the singular physical and chemical properties of materials filled in tubes, and are expected to be applied to thefields of catalysis, biology, medicine and the like.

Description

technical field [0001] The invention relates to the field of structure-controlled preparation of single-wall carbon nanotubes, in particular to a macroscopic and controllable preparation method of large-diameter and narrow-diameter distribution single-wall carbon nanotubes. Background technique [0002] Carbon nanotubes have nanoscale one-dimensional hollow lumens. In the nanoscale local space, the arrangement of guest molecules may be completely different from the macroscopic surface, and many extreme physical and chemical processes can occur. Therefore, carbon nanotubes are also considered to be the smallest "Chemical Test Tubes". Since its discovery, the huge aspect ratio of carbon nanotubes and the nearly ideal one-dimensional nano-hollow lumen have aroused great interest among chemists. The hollow lumen of carbon nanotubes is predicted to be used as nano-test tubes, siphons, super Adsorbents, catalyst supports, energy storage materials, electrode materials, etc. [00...

Claims

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Application Information

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IPC IPC(8): C01B32/159C01B32/16
CPCC01B32/159C01B32/16C01B2202/36Y02P20/52
Inventor 侯鹏翔石超刘畅成会明
Owner 唯碳纳米科技(沈阳)有限公司
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