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Preparation method and application of carbon nanofibers

A carbon nanofiber and nanofiber membrane technology, applied in the field of carbon nanofiber preparation, can solve the problems of difficult control, cumbersome processing steps, inability to greatly improve the electrochemical performance of electrodes, etc. The effect of simple and easy process

Inactive Publication Date: 2019-08-16
TIANJIN POLYTECHNIC UNIV
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  • Claims
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Problems solved by technology

[0004] At present, there are three main methods of activating carbon nanofibers: the first method is gas activation, which continues to maintain high temperature after carbonization, and introduces carbon dioxide gas, using carbon dioxide to react with carbon at high temperature to generate pores and increase its specific surface area. ; The carbon nanofibers obtained by this method are micropores (size<2nm), compared with mesoporous (2-50nm), micropores can not greatly improve the electrochemical performance of the electrode; the second method is acid-base Salt activation, carbon nanofibers are mixed with phosphoric acid, potassium hydroxide or zinc chloride and then activated at high temperature. This method will produce a large number of mesopores, but the activated carbon nanofibers need to be subsequently neutralized. The method is not easy to control, the yield is low, the process is complex and will produce certain pollution; the third method is in-situ activation, that is, adding inorganic fillers, such as calcium carbonate, zinc oxide, etc., when preparing the spinning precursor, using inorganic fillers Pyrolysis produces pores during carbonization. This method needs to remove impurities (such as calcium oxide and zinc oxide) remaining in carbon nanofibers, and the subsequent processing steps are cumbersome.

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  • Preparation method and application of carbon nanofibers
  • Preparation method and application of carbon nanofibers
  • Preparation method and application of carbon nanofibers

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preparation example Construction

[0026] The invention provides a method for preparing carbon nanofibers, comprising the following steps:

[0027] Mix carbon source, starch and organic solvent to obtain precursor solution;

[0028] Electrospinning the precursor solution to obtain a nanofibrous membrane;

[0029] The nanofiber film is subjected to pre-oxidation treatment and carbonization treatment in sequence to obtain carbon nanofibers.

[0030] The invention mixes carbon source, starch and organic solvent to obtain precursor solution. In the present invention, the carbon source preferably includes one or more of polyacrylonitrile, pitch, lignin, phenolic resin, polyimide and polybenzimidazole, more preferably polyacrylonitrile, lignin or Polyimide, most preferably polyacrylonitrile. In the present invention, the starch preferably includes one or more of high amylose, high amylopectin and potato starch, more preferably high amylose or high amylopectin. In the present invention, the mass ratio of the carbo...

Embodiment 1

[0045] Mix polyacrylonitrile (PAN) and starch (mass ratio of polyacrylonitrile to starch: 8:2), dissolve in dimethyl sulfoxide, place in a conical flask, stir in a water bath at 60°C for 24h, Get a precursor solution with a total mass concentration of 10%, put the precursor solution into a syringe for standby; paste aluminum foil paper on the drum of the electrospinning machine, and set the spinning parameters: the receiving distance is 15cm, and the advancing speed is 1mL / h, the voltage is 20kV, the drum speed is 100rpm, and the ambient temperature is controlled at 40°C, and the precursor solution is electrospun to obtain a nanofiber film;

[0046] The nanofiber membrane is subjected to pre-oxidation treatment and carbonization treatment, and the parameters of the pre-oxidation process are set as follows: in the air environment, the temperature is raised to 260 ° C at a heating rate of 2 ° C / min, and the temperature is maintained for 60 min; the carbonization process parame...

Embodiment 2

[0058] Mix polyimide and starch (mass ratio of polyacrylonitrile to starch: 7:3) and dissolve in dimethyl sulfoxide, place in an Erlenmeyer flask, stir in a water bath at 50°C for 10 hours, and obtain the total mass Precursor solution with a concentration of 9%, put the precursor solution into a syringe for standby; paste aluminum foil paper on the drum of the electrospinning machine, and set the spinning parameters: the receiving distance is 20cm, and the advancing speed is 1.5mL / h , the voltage is 18kV, the drum speed is 150rpm, and the ambient temperature is controlled at 50°C, and the precursor solution is electrospun to obtain a nanofiber film;

[0059] The nanofiber membrane is subjected to pre-oxidation treatment and carbonization treatment, and the parameters of the pre-oxidation process are set as follows: in the air environment, the temperature is raised to 240 ° C at a heating rate of 3 ° C / min, and the temperature is kept for 30 min; the carbonization process para...

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Abstract

The invention belongs to the technical field of electrode materials, in particular to a preparation method and an application of carbon nanofibers. In the preparation process of carbon nanofibers, starch used as a pore forming agent is decomposed at a lower temperature (200-300 DEG C), and starch is decomposed in the pre-oxidation stage. After pre-oxidation and carbonization, a large number of micro-pores and mesopores will be produced with the shrinkage of fibers. Thus, the specific surface area and the porosity of the carbon nanofibers are greatly improved. When the carbon nanofibers prepared are used to make super capacitors, the specific capacitance of super capacitors can reach 70F / g, which shows that the carbon nanofibers prepared in the invention have excellent electrochemical performance.

Description

technical field [0001] The invention relates to the technical field of electrode materials, in particular to a preparation method and application of carbon nanofibers. Background technique [0002] Carbon nanofiber is a nano-sized carbon-based material obtained by electrospinning technology from polymer precursors, followed by pre-oxidation and carbonization. Carbon nanofibers have excellent nanostructure, high degree of graphitization and stable physical and chemical structure, and are good electrode materials for supercapacitors. But after pre-oxidation and carbonization, pure carbon nanofibers do not produce a rich pore structure, so carbon nanofibers have low specific surface area and porosity. [0003] The principle of carbon-based supercapacitor is the principle of electric double layer, which mainly uses the adsorption of the electrode to the electrolyte to increase the electrochemical performance. Therefore, in order to improve the electrochemical performance of su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G11/36H01G11/24H01G11/44H01G11/34H01G11/86
CPCH01G11/24H01G11/34H01G11/36H01G11/44H01G11/86Y02E60/13
Inventor 王闻宇王赫王洪杰金欣郑意德
Owner TIANJIN POLYTECHNIC UNIV
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