A kind of preparation method of large-area nitrogen-doped carbon nanotube paper

A carbon nanotube and nanotube technology, which is applied in the field of large-area nitrogen-doped carbon nanotube paper and its preparation, can solve the problems of control method limitation, complex preparation process, and difficulty in meeting the requirements, and achieves simple equipment and strong controllability and operability. , the effect of easy direct application and batch preparation

Active Publication Date: 2017-12-12
SUN YAT SEN UNIV
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Problems solved by technology

[0004] In the existing methods, many need to use substrates to regulate the growth of nanotubes to obtain nitrogen-doped carbon nanotubes with specific properties. The preparation process is not only complicated, but also the regulation methods are limited.
Not only that, the existing preparation process is also difficult to directly obtain large-area nitrogen-carbon nanotubes, so it increases certain difficulties in actual industrial production, and it is difficult to meet the needs of modern industry and technological development.

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  • A kind of preparation method of large-area nitrogen-doped carbon nanotube paper
  • A kind of preparation method of large-area nitrogen-doped carbon nanotube paper
  • A kind of preparation method of large-area nitrogen-doped carbon nanotube paper

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preparation example Construction

[0035] The invention adopts CVD method to prepare large-area nitrogen-doped carbon nanotube paper. The preparation method of the nitrogen-doped carbon nanotube paper comprises the following steps:

[0036] 1) take by weighing ferrocene powder ((C 5 h 5 ) 2 Fe) dissolved in dichlorobenzene (C 6 h 4 Cl 2 ), it is prepared into a ferrocene / dichlorobenzene carbon source solution with a concentration of 20-150mg / mL; measure a certain amount of pyridine (C 5 h 5 N) mixed with ferrocene / dichlorobenzene carbon source solution to form ferrocene / dichlorobenzene / pyridine mixed carbon source solution, the ratio of pyridine to dichlorobenzene is controlled at 1:1~1:2;

[0037] 2) Curl the base of the iron sheet or copper sheet into a cylindrical shape and put it into the quartz reaction chamber of the reaction furnace, and make it as close as possible to the inner wall of the quartz reaction chamber to seal the reaction chamber, and flow argon with a flow rate of 100-500mL / min into ...

Embodiment 1

[0043] Weigh 4.0g of ferrocene powder and dissolve it in 100mL of dichlorobenzene to prepare a ferrocene / dichlorobenzene carbon source solution with a concentration of 40mg / mL; measure 1mL of pyridine and 10ml of ferrocene / dichlorobenzene carbon The source solutions are mixed to form a ferrocene / dichlorobenzene / pyridine mixed carbon source solution, and the ratio of pyridine to dichlorobenzene is 1:10.

[0044]Ultrasonic the copper sheet with the size of 18cm×20cm×0.1cm for 15 minutes, curl it into a cylindrical shape and put it into the quartz reaction chamber of the reaction furnace, and make it as close as possible to the inner wall of the quartz reaction chamber to seal the reaction chamber, and to the reaction chamber Introduce argon gas with a flow rate of 100mL / min to exhaust the air in the reaction chamber, and heat the reaction furnace at the same time; Hydrogen, forming argon hydrogen mixed carrier gas.

[0045] Use a precision syringe pump to inject the ferrocene / d...

Embodiment 2

[0049] Weigh 4.0g of ferrocene powder and dissolve it in 100mL of dichlorobenzene to prepare a ferrocene / dichlorobenzene carbon source solution with a concentration of 40mg / mL; measure 1mL of pyridine and 5ml of ferrocene / dichlorobenzene carbon The source solutions are mixed to form a ferrocene / dichlorobenzene / pyridine mixed carbon source solution, and the ratio of pyridine to dichlorobenzene is 1:5.

[0050] Ultrasonic the copper sheet with the size of 18cm×20cm×0.1cm for 15 minutes, curl it into a cylindrical shape and put it into the quartz reaction chamber of the reaction furnace, and make it as close as possible to the inner wall of the quartz reaction chamber to seal the reaction chamber, and to the reaction chamber Introduce argon gas with a flow rate of 100mL / min to exhaust the air in the reaction chamber, and heat the reaction furnace at the same time; Hydrogen, forming argon hydrogen mixed carrier gas.

[0051] Use a precision syringe pump to inject the ferrocene / di...

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Abstract

The invention provides a large area nitrogen-doped carbon nano-tube paper preparation method, which comprises: (1) weighing ferrocene powder, dissolving in dichlorobenzene to form a ferrocene / dichlorobenzene carbon source solution, weighing pyridine, and mixing the pyridine and the ferrocene / dichlorobenzene carbon source solution to form a ferrocene / dichlorobenzene / pyridine mixing carbon source solution; 2) coiling an iron sheet or copper sheet substrate into a cylindrical material, placing into the quartz reaction chamber of a reaction furnace, sealing the reaction chamber, introducing argon gas to completely discharge air, and heating the reaction furnace; 3) when the temperature of the reaction chamber achieves 750-900 DEG C, adjusting the argon flow rate while introducing hydrogen; 4) injecting the ferrocene / dichlorobenzene / pyridine mixing carbon source solution into the reaction chamber, and carrying out a reaction; and 5) stopping the heating of the tubular reaction furnace, closing the hydrogen, adjusting argon flow rate to make the product be cooled to a room temperature along with the furnace, and collecting the large area nitrogen-doped carbon nano-tube paper on the substrate. According to the present invention, the nitrogen-doped structure carbon nano-tube film two-dimensional structure and the simple, rapid and large-scale preparation method can be used for the fields of new energy sources, sensors, flexible electronic devices, and the like.

Description

technical field [0001] The invention relates to a nitrogen-doped carbon nanotube paper two-dimensional material, which belongs to the technical field of nano-carbon material preparation, in particular to a large-area nitrogen-doped carbon nanotube paper and its preparation method, which is used in new energy, sensors and flexible It has important applications in electronic devices and other fields. Background technique [0002] Since Ijima discovered carbon nanotubes in 1991, scientists have increasingly recognized the important role of carbon nanotubes in scientific development and human progress. Carbon nanotubes, as the most typical one-dimensional nanomaterials, exhibit excellent and unique electrical, mechanical, electrochemical and other properties. Carbon nanotubes are also ideal units for building macroscopic materials. Carbon nanotube paper (also known as Bucky paper, BP, Bucky paper), which occupies an important position in carbon nanotube macroscopic materials, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/16B82Y40/00
CPCC01P2002/85C01P2004/01C01P2004/03
Inventor 桂许春郑永嘉林志强汤子康
Owner SUN YAT SEN UNIV
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