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A graphene-reinforced preparation method of micro-nano film-like carbon fibers

A technology of graphene and carbon fiber, which is applied to the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of carbon fiber strength stagnation, defects, and difficulty in reducing the diameter of carbon fiber precursors, and achieve good traction and stretching of fibers, improving strength and performance , the effect of reducing defects and holes

Active Publication Date: 2021-06-15
孙旭阳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is difficult for the traditional spinning technology to make the single filament diameter less than 2 μm according to the requirements of the carbon fiber precursor, and the too fine fiber brings great difficulties to processes such as mechanical stretching.
Without sufficient "fine denier", it is difficult to reduce the reduction of defect holes, so the improvement of carbon fiber strength has stagnated in recent years
[0010] 2. It is difficult to reduce the diameter of carbon fiber precursors to microns or below, and the "skin-core structure" of carbon fibers is unavoidable
[0012] 3. It is difficult to reduce the diameter of carbon fiber precursors to microns or below. In order to prevent the diffusion and "double diffusion" channels from increasing and expanding, the process is slow and complicated, resulting in long process and low production efficiency
[0013] 4. The diameter of carbon fiber is relatively large, so it is difficult to adopt advanced heating methods such as electric induction
The traditional heating method has low thermal efficiency, long process time and large loss of raw materials, resulting in high cost of carbon fiber
[0014] 5. If the substrate is coated with a micronano-thick polymer coating and spun into a micronano-thick silk film, thermal stabilization (pre-oxidation, non-melting and heat treatment), carbonization, graphitization, and formation of micro-nano films Shaped carbon fiber, although the "fine denier" of carbon fiber can be realized, but the metal on the base material will form carbides with the carbon fiber during the high temperature process of the process, causing defects and affecting the improvement of carbon fiber performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] (1) Preparation of spinning stock solution:

[0058] Polyacrylonitrile-based spinning dope: monomer acrylonitrile (AN), second monomer itaconic acid (ITA), third monomer methyl acrylate (MAA), initiator azobisisobutyronitrile (AIBN) according to After the ratio of 96:1:3:0.2, it is polymerized to form a terpolymer (PAN) solution, and then mixed with the solvent dimethyl sulfoxide (DMSO) in a ratio of 1:9 to make a spinning stock solution.

[0059] (2) Graphene substrate grown by CVD method: nickel metal wire with a diameter of 10 μm, in a hydrogen and nitrogen protective atmosphere, using methane as a carbon raw material, and growing 1 to 10 layers of graphene at a growth temperature of 950 to 1000 ° C, After cooling, it serves as a graphene-enhanced substrate.

[0060] (3) Spinning and film forming process: the above-mentioned substrate is drawn and immersed in the tank containing the spinning stock solution, and then pulled out evenly at a speed of 10m / s to form a 0....

Embodiment 2

[0066] (1) Preparation of spinning stock solution:

[0067] Polyacrylonitrile-based spinning dope: monomer acrylonitrile (AN), second monomer itaconic acid (ITA), third monomer methyl acrylate (MAA), initiator azobisisobutyronitrile (AIBN) according to After the ratio of 96:1:3:0.2, it is polymerized to form a terpolymer (PAN) solution, and then mixed with the solvent dimethyl sulfoxide (DMSO) in a ratio of 1:9 to make a spinning stock solution.

[0068] (2) Graphene substrate grown by CVD method: nickel metal wire with a diameter of 10 μm, in a hydrogen and nitrogen protective atmosphere, using methane as a carbon raw material, and growing 1 to 10 layers of graphene at a growth temperature of 950 to 1000 ° C, After cooling, it serves as a graphene-enhanced substrate.

[0069] (3) Spinning and film forming process: the above-mentioned substrate is drawn and immersed in the tank containing the spinning stock solution, and then pulled out evenly at a speed of 10m / s to form a 0....

Embodiment 3

[0076] (1) Preparation of spinning stock solution:

[0077] Pitch-based spinning dope: Spinning dope is made from mesophase pitch melt.

[0078] (2) Growth of graphene substrate by CVD method: using a hollow refined copper tube with an inner diameter of 3mm and a thickness of 30μm, in a hydrogen and nitrogen protective atmosphere, methane is used as the carbon raw material, and a growth temperature of 950-1000°C is used to grow 1- 10 layers of graphene, cooled as a graphene-enhanced substrate.

[0079] (3) Spinning film-forming process: the above-mentioned base material is dipped into the tank containing the spinning stock solution by traction, and then pulled out evenly at a speed of 20m / s to form a mesophase pitch liquid film of 0.3-0.5μm. Stretching, the liquid film is cooled and solidified into a silk film in the air while obtaining good orientation.

[0080] (3) Non-melting process: introduce the obtained fiber coated with pitch silk film into a non-melting furnace for ...

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Abstract

A graphene-reinforced preparation method for micro-nano film-like carbon fibers, characterized in that, using metal filaments or hollow metal thin-walled tubes as substrates, graphene is grown by CVD as a graphene-reinforced substrate, and the prepared spinning stock solution is passed through After polymerization, evenly coat the above-mentioned graphene-enhanced substrate to form a polymer coating with a thickness of micronano; spin into a silk film with a thickness of micronano; then thermally stabilize it by means of electric induction heating supplemented by auxiliary heating and carbonization to form a carbon film, and the carbon film and the substrate form a composite micro-nano film-shaped graphene-reinforced carbon fiber; the substrate is removed to form a simple micro-nano-film-shaped graphene-reinforced carbon fiber; the above-mentioned simple micro-nano-film-shaped carbon fiber is used as the substrate According to the above-mentioned process, the laminated micro-nano film-like graphene-reinforced carbon fiber can be prepared repeatedly. The micro-nano film-like carbon fiber structure and the preparation method thereof of the present invention can significantly improve the performance of the carbon fiber, improve the structure of the carbon fiber, increase the production efficiency and reduce the manufacturing cost.

Description

technical field [0001] The invention relates to carbon fiber technology, in particular to a graphene-reinforced preparation method of micro-nano film-like carbon fibers. Background technique [0002] Carbon fiber (CF for short) is a new type of fiber material with high strength and high modulus fibers with a carbon content of more than 95%. It is a microcrystalline graphite material stacked along the axial direction of the fiber by carbonizing and graphitizing organic fibers. [0003] Carbon fiber has two characteristics of strong tensile strength of carbon material and soft processability of fiber. It is a new material with excellent mechanical and electrical properties. At present, the tensile strength of mass-produced carbon fibers is about 2 to 7 GPa, and the tensile modulus is about 200 to 700 GPa. The density is about 1.5 to 2.0 grams per cubic centimeter. Generally, after graphitization treatment at a high temperature of 3000 ° C, the density can reach 2.0 grams per...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/14D01F9/22D01F9/145
CPCD01F9/14D01F9/145D01F9/22
Inventor 孙旭阳
Owner 孙旭阳