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Preparation method and carbon fiber material with controllable pore size and porosity of carbon fiber material

A carbon fiber material and porosity technology, applied in the field of porous carbon material preparation, can solve the problems of complex purification process, small fiber length, inability to prepare continuous fiber, etc., and achieve the effect of easy operation method and simple preparation method

Active Publication Date: 2018-02-06
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the vapor phase growth method is the most common, but the carbon nanofibers prepared by this method show many disadvantages: (1) the fiber length is too small to prepare continuous fibers; (2) the obtained fiber products contain a large amount of metal due to the necessity of using a catalyst. Impurities require complex purification processes; (3) high equipment costs are not conducive to industrial production

Method used

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  • Preparation method and carbon fiber material with controllable pore size and porosity of carbon fiber material
  • Preparation method and carbon fiber material with controllable pore size and porosity of carbon fiber material
  • Preparation method and carbon fiber material with controllable pore size and porosity of carbon fiber material

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Effect test

Embodiment 1

[0039] Polyacrylonitrile with a molecular weight of 150,000 and SiO with a particle size of 200nm 2 The microspheres were dissolved in N,N-dimethylformamide (DMF) at a mass ratio of 17:1, stirred magnetically at 1000rpm for 5h, and then prepared SiO by electrospinning technology. 2 - Polyacrylonitrile fiber, the process parameters of electrospinning are as follows: voltage 20kV, pushing speed 2mL / h, the distance between the needle tip and the receiver is 15cm, and the receiver is copper foil.

[0040] SiO 2 -Polyacrylonitrile fibers soaked in 10wt% hydrofluoric acid solution to remove SiO 2 The microspheres were then washed with absolute ethanol and deionized water. Then heated to 300°C at a heating rate of 1°C / min in an air atmosphere, and kept for 1 hour; then heated to 800°C at a heating rate of 1°C / min in a nitrogen atmosphere, kept for 1 hour, and the pore size of 200nm was obtained after cooling down. carbon fiber material.

[0041] figure 1 The SEM image of the car...

Embodiment 2

[0044] The polyacrylonitrile that molecular weight is 50000 is dissolved in methylpyrrolidone (NMP) obtains the polyacrylonitrile solution that mass fraction is 10%, the SiO that particle diameter is 100nm 2 The microspheres were dissolved in methylpyrrolidone (NMP) to obtain SiO with a mass fraction of 5% 2 suspension, then take 4.75g polyacrylonitrile solution and 0.5g SiO 2 The suspension was mixed, stirred magnetically at 1000rpm for 3h, and then prepared SiO by electrospinning 2 - Polyacrylonitrile fiber, the process parameters of electrospinning are as follows: voltage 15kV, pushing speed 1mL / h, the distance between the needle tip and the receiver is 15cm, and the receiver is copper foil.

[0045] Then heated to 300°C at a heating rate of 5°C / min under an air atmosphere, and kept for 1 hour; then heated to 1000°C at a heating rate of 1°C / min under a nitrogen atmosphere, kept for 1 hour, and soaked in a concentration of 10wt% after cooling. Hydrofluoric acid solution to...

Embodiment 3

[0047] Dissolving polyacrylonitrile with a molecular weight of 23000 in N,N-dimethylformamide (DMF) to obtain a polyacrylonitrile solution with a mass fraction of 10%, SiO with a particle size of 50nm 2 The microspheres were dissolved in N,N-dimethylformamide (DMF) to obtain 5% SiO 2 suspension, then take 4.75g polyacrylonitrile solution and 0.5g SiO 2 The suspension was mixed, stirred magnetically at 1000rpm for 5h, and then prepared SiO by electrospinning 2 - Polyacrylonitrile fiber, the process parameters of electrospinning are as follows: voltage 20kV, pushing speed 2mL / h, the distance between the needle tip and the receiver is 15cm, and the receiver is copper foil.

[0048] Then heated to 200°C at a heating rate of 0.5°C / min in an air atmosphere, and kept for 1 hour; then heated to 700°C at a heating rate of 1°C / min in a nitrogen atmosphere, kept for 1 hour, and continued at a heating rate of 5°C / min The temperature was raised to 1100°C at a certain rate and kept for 2 ...

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Abstract

The invention discloses a preparation method of a carbon fiber material with adjustable pore diameter and porosity and the carbon fiber material. The preparation method comprises following steps: SiO2-polyacrylonitrile fibers are prepared with an electrospinning technique; the SiO2-polyacrylonitrile fibers are soaked in a hydrofluoric acid solution, SiO2 in the SiO2-polyacrylonitrile fibers is removed, and the fibers are washed with absolute ethyl alcohol and deionized water; the fibers are subjected to pre-oxidation for 1-6 h at the temperature of 150-400 DEG C under the air atmosphere, then an obtained product is subjected to carbonization for 0.5-8 h at the temperature of 600-1,500 DEG C under the inert gas atmosphere, and the carbon fiber material is obtained after cooling. According to the preparation method, the carbon fiber material with adjustable pore diameter and porosity is obtained through adjustment of grain size and mass fraction of SiO2 microspheres; the preparation method is simple, and the operation method is easy.

Description

technical field [0001] The invention belongs to the field of porous carbon material preparation, and in particular relates to a preparation method and a carbon fiber material capable of regulating the aperture and porosity of a carbon fiber material. Background technique [0002] Electrospinning is a method of using a high-voltage electrostatic field to act on a polymer solution or molten liquid to obtain nanometer-scale (50-500nm) polymer nanofibers. This method originates from the patent (US 1975504,1934) of American Formhals. The fiber diameters produced by traditional spinning techniques (such as dry spinning, wet spinning, melt spinning, etc.) are in the range of tens to hundreds of microns; while other preparation methods of several polymer nanofibers, such as template synthesis method (Feng L, Li S, Li H, etal.Angew Chem Int Ed, 2002, 41:1221~1223), phase separation method (Ma P X, Zhang R.J Biomed MatRes, 1999, 46:60~72), self-assembly The method (Whitesides G M, G...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/22D01F6/54D01F1/02D01F11/12D01D5/00
CPCD01D5/003D01F1/02D01F6/54D01F9/22D01F11/121
Inventor 倪伟王斌杨丹程建丽李小东
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS