Preparation method of nitrogen-doped carbon nanotube thin film having high electrochemical properties

A nitrogen-doped carbon, electrochemical technology, applied in the direction of circuits, electrical components, battery electrodes, etc., can solve the problems of complicated process and difficult to realize large-scale industrial production, and achieve the effect of simple operation, increased capacity, and improved capacity

Inactive Publication Date: 2015-07-15
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the disadvantages of the prior art that the process is complicated and it is difficult to realize large-scale industrial production, and to provide a nitrogen-doped carbon nanotube thin film lithium with simple operation, easy to realize large-scale preparation and high electrochemical performance. Preparation method of ion battery negative electrode material

Method used

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  • Preparation method of nitrogen-doped carbon nanotube thin film having high electrochemical properties
  • Preparation method of nitrogen-doped carbon nanotube thin film having high electrochemical properties
  • Preparation method of nitrogen-doped carbon nanotube thin film having high electrochemical properties

Examples

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Effect test

Embodiment 1

[0026] (1) Take by weighing 25g of ethanol as a carbon source, 0.25g of ferrocene as a catalyst, 0.2g of thiophene as a promotor, and add 1.25g of ammonia as a nitrogen source, mix and sonicate for 30min; obtain a uniform precursor solution; The mass ratio of carbon source ethanol and nitrogen source ammonia water is 100:5;

[0027] (2) A vertical furnace is used as the reactor. The reactor is heated to 1100°C under the protection of argon and then kept warm. The carrier gas is replaced by argon with hydrogen (the gas flow rate is 600 sccm), and then the prepared precursor solution is 8mL h -1 The rate is injected into the reactor;

[0028] (3) After the reaction starts, when a cylindrical film is formed at the tail end of the reactor, it is drawn to the rotating shaft to obtain a uniform and continuous film;

[0029] (4) After the reaction, heat-treat the collected film at 400° C. for 2 h under air condition to remove amorphous carbon in the product, and finally obtain the ...

Embodiment 2

[0032] (1) Take 25g of ethanol as a carbon source, 0.25g of ferrocene as a catalyst, 0.2g of thiophene as a promotor, and add 2.5g of ammonia as a nitrogen source, mix and sonicate for 30min; obtain a uniform precursor solution; The mass ratio of carbon source ethanol and nitrogen source ammonia water is 100:10;

[0033] (2) A vertical furnace is used as the reactor. The reactor is heated to 1100°C under the protection of argon and then kept warm. The carrier gas is replaced by argon with hydrogen (the gas flow rate is 600 sccm), and then the prepared precursor solution is 8mL h -1 The rate is injected into the reactor;

[0034] (3) After the reaction starts, when a cylindrical film is formed at the tail end of the reactor, it is drawn to the rotating shaft to obtain a uniform and continuous film;

[0035] (4) After the reaction, heat-treat the collected film at 400° C. for 2 h under air condition to remove amorphous carbon in the product, and finally obtain the nitrogen-dop...

Embodiment 3

[0038] (1) Take by weighing 25g of ethanol as a carbon source, 0.25g of ferrocene as a catalyst, 0.2g of thiophene as a promotor, and add 1.25g of ethanolamine as a nitrogen source, mix and sonicate for 30min; obtain a uniform precursor solution; The mass ratio of carbon source ethanol and nitrogen source ethanolamine is 100:5;

[0039] (2) A vertical furnace is used as the reactor. The reactor is heated to 1100°C under the protection of argon and then kept warm. The carrier gas is replaced by argon with hydrogen (the gas flow rate is 600 sccm), and then the prepared precursor solution is 8mL h -1 The rate is injected into the reactor;

[0040] (3) After the reaction starts, when a cylindrical film is formed at the tail end of the reactor, it is drawn to the rotating shaft to obtain a uniform and continuous film;

[0041] (4) After the reaction, heat-treat the collected film at 400° C. for 2 h under air condition to remove amorphous carbon in the product, and finally obtain ...

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Abstract

The invention provides a preparation method of a nitrogen-doped carbon nanotube thin film having high electrochemical properties and discloses a preparation method of an anode material of a nitrogen-doped carbon nanotube lithium-ion battery. The following floating catalytic chemical vapor deposition method is adopted: a liquid-phase carbon source, a nitrogen source, a catalyst and an accelerant are mixed and then ultrasonically dispersed to obtain an even precursor solution; a reactor is heated to the range of 900-1200 DEG C in an argon environment and kept at a constant temperature, under the driving of a carrier gas (hydrogen or hydrogen and argon mixed gas), and the precursor solution is injected into the reactor at the rate of 2-12mL/h, then a uniform and continuous thin film can be obtained; the thin film is thermally treated for 1-4 hours under the air condition of 300-600 DEG C, and finally, the anode material of the nitrogen-doped carbon nanotube lithium-ion battery is obtained. The preparation method is simple in process, relatively low in energy consumption, and capable of further improving the properties of the material; under the current density of 30mAg<-1>, the initial charge capacity and the initial discharge capacity of the material are 591.1mAhg<-1> and 1644.4mAhg<-1>, respectively; after 100 charge-discharge cycles under the current density of 3000mAg<-1>, the charge capacity and the discharge capacity are stabilized at 293.2mAhg<-1> and 305.1mAhg<-1>; in short, the preparation method can be widely applied to the electrode materials of the lithium ion batteries.

Description

technical field [0001] The invention relates to lithium-ion battery negative electrode materials, in particular to a preparation method for a nitrogen-doped carbon nanotube film with high electrochemical performance. Background technique [0002] Due to its unique hollow structure, high specific surface area, good electrical conductivity, remarkable mechanical, electrochemical and field emission properties, carbon nanotubes have attracted widespread attention in many fields, especially their use as energy storage materials has greatly Promote the development of supercapacitors and lithium-ion batteries. In recent years, the application performance of carbon nanotubes has been improved by doping carbon nanotubes with nitrogen, which has become one of the research hotspots in the field of carbon nanotube synthesis and application. Doping carbon nanotubes with nitrogen can change the local charge density of carbon nanotubes, improve the electron transport of carbon nanotubes, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1393H01M4/139
CPCH01M4/139H01M4/1393Y02E60/10
Inventor 侯峰杨德明
Owner TIANJIN UNIV
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