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A method for controllable growth of metallic single-walled carbon nanotubes through substrate design

A single-wall carbon nanotube, carbon nanotube technology, applied in the direction of carbon nanotubes, nanocarbons, non-metallic elements, etc., can solve the problems of poor high temperature thermal stability, poor uniformity of carbon nanotube diameter, poor repeatability, etc. Effects of large growth rate differences

Active Publication Date: 2022-08-09
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] However, there are still many problems in the preparation of metallic single-walled carbon nanotubes: (1) The catalyst has poor thermal stability at high temperature on the surface of the silicon substrate with which it interacts less, resulting in poor uniformity of carbon nanotube diameter; (2) It is difficult to control the crystal plane structure and symmetry of the catalyst, resulting in poor repeatability; (3) The mechanism of the controllable growth of metallic single-walled carbon nanotubes is still unclear; (4) The substrate directly affects the growth of carbon nanotubes. Thermodynamic and kinetic factors are unclear

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  • A method for controllable growth of metallic single-walled carbon nanotubes through substrate design
  • A method for controllable growth of metallic single-walled carbon nanotubes through substrate design
  • A method for controllable growth of metallic single-walled carbon nanotubes through substrate design

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Effect test

Embodiment 1

[0046] In this embodiment, the spinel containing the (110) crystal plane treated in the above step (1) is heat-treated at 450° C. for 3 hours in the air.

[0047] Adopt step (2) to support the cobalt particles on the spinel (110) surface and carry out oxidation and reduction treatment, the oxidation conditions are 450 ℃, 3min; the reduction conditions are 765 ℃, 90sccmAr+4sccmH 2 , 3min. The morphology of the cobalt particles prepared in step (2) was characterized by transmission electron microscopy ( Figure 5 a), the particle size was found to be small and uniform; the diameter distribution of cobalt particles under the transmission electron microscope ( Figure 5 b) shows that the particle size is mainly concentrated in 1-3 nm; Figure 5 Scanning transmission electron imaging of c further demonstrates the compositional homogeneity of the cobalt particles. The surface of the substrate was sputtered by X-ray photoelectron spectroscopy and secondary ion mass spectrometry, r...

Embodiment 2

[0050] In this embodiment, step (1) is the same as step (1) of the embodiment, and the temperature and time of heat treatment in air are 500° C. and 2h, respectively.

[0051] Step (2) is the same as the step (2) of the embodiment, the oxidation temperature and time are respectively 600 ℃, 1min, the reduction temperature and time are respectively 850 ℃, 1min, and the reducing atmosphere is 100sccmAr+3sccmH 2 . The size and morphology of the Co particles were characterized by transmission electron microscopy. The lattice fringe spacing of the 50 particles is centered at 0.2-0.22 nm, indicating that the substrate has a significant effect of stabilizing the catalyst structure.

[0052]Step (3) is the same as the step (3) of the embodiment, the growth temperature and time of the single-walled carbon nanotubes are respectively 775 ° C and 7min, the argon flow rate loaded with ethanol is 17sccm, the hydrogen flow rate is 1sccm, and the argon carrier gas flow rate is 90sccm. Scann...

Embodiment 3

[0054] In this embodiment, step (1) is the same as step (1) of the embodiment, and the temperature and time of heat treatment in air are 400° C. and 3h, respectively.

[0055] Step (2) is the same as the step (2) of the embodiment, the oxidation temperature and time are respectively 400 ℃, 5min, the reduction temperature and time are respectively 700 ℃, 5min, and the reducing atmosphere is 80sccmAr+5sccmH 2 . The size and morphology of the Co particles were characterized by transmission electron microscopy. The lattice fringe spacing of the 50 particles is centered at 0.2-0.22 nm, indicating that the substrate has a significant effect of stabilizing the catalyst structure.

[0056] Step (3) is the same as the step (3) of the embodiment, the growth temperature and time of the single-walled carbon nanotubes are respectively 765 ° C and 10min, the argon flow rate loaded with ethanol is 20sccm, the hydrogen flow rate is 3sccm, and the argon carrier gas flow rate is 100sccm. Sca...

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Abstract

The invention relates to the field of controllable preparation of metallic single-walled carbon nanotubes, in particular to a method for controllably growing metallic single-walled carbon nanotubes through substrate design. Using spinel as the substrate, metal oxide nanoclusters with uniform size were prepared by self-assembly method of block copolymer; the size, structure and high temperature stability of catalyst nanoparticles were regulated by the solid solution and pinning effect of spinel substrate on catalyst nanoparticles. Combined with the effect of spinel substrate on the growth rate of single-walled carbon nanotubes with different conductive properties, the selective growth of metallic single-walled carbon nanotubes is achieved. The prepared metallic single-walled carbon nanotubes have a diameter of 1.1±0.2 nm and a content of 75-85 percent. The invention realizes the direct and controllable growth of metallic single-walled carbon nanotubes with narrow diameter distribution through substrate design and selection, and lays a material foundation for promoting the application of metallic single-walled carbon nanotubes.

Description

technical field [0001] The invention relates to the field of controllable preparation of metallic single-walled carbon nanotubes, in particular to a method for controllably growing metallic single-walled carbon nanotubes through substrate design. Background technique [0002] Single-walled carbon nanotubes can be metallic or semiconducting due to their different chiral angles and diameters. Metallic single-walled carbon nanotubes with quantum transport effects can be used as flexible electrode materials and interconnecting wires for future nanoelectronic devices. However, commonly prepared SWCNT samples are a mixture of metallic and semiconducting carbon tubes. How to obtain high-purity metallic single-walled carbon nanotubes is the key to promote their practical application. The content of metallic single-walled carbon nanotubes in common samples is only about 1 / 3, and its chemical activity is higher than that of semiconducting single-walled carbon nanotubes, so it is mor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/159C01B32/162
CPCC01B32/159C01B32/162C01B2202/34C01B2202/36
Inventor 刘畅李鑫张峰侯鹏翔张莉莉成会明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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