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Method for preparing high-intensity high-modulus graphite fibers

A graphite fiber and high modulus technology, applied in the field of carbon fiber, can solve problems such as insufficient pre-oxidation, carbon fiber performance degradation, fusion, etc., and achieve a good guiding effect

Active Publication Date: 2015-07-29
WEIHAI TUOZHAN FIBER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Insufficient pre-oxidation, pre-oxidized fibers are prone to fusion during the carbonization stage, resulting in reduced performance of carbon fibers
Excessive pre-oxidation, excessive oxygen elements combined on the PAN molecular chain, oxygen in the process of carbonization with H 2 O, CO, CO 2 The escape of the small molecular form will also lead to a decrease in the performance of carbon fibers

Method used

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  • Method for preparing high-intensity high-modulus graphite fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Wet-spun Weihai Extension Fiber Co., Ltd. produced PAN copolymer fibers containing more than 90% acrylonitrile monomer components (the tow is 12K, and the copolymer composition (wt%) is: acrylonitrile (AN): Methyl acrylate (MA): itaconic acid (IA) = 96:2:2), in air medium, adopt six stages of pre-oxidation treatment at 190°C, 210°C, 220°C, 230°C, 245°C, 255°C, The residence time is 90min, the draw ratio is 1%, and the obtained density is 1.32g / cm 3 The pre-oxidized fiber, under the protection of nitrogen, the pre-oxidized fiber is subjected to low-temperature carbonization at a temperature of 300-900°C, the residence time is 3min, and a +2% draft ratio is applied; a -3% draft is applied at a temperature of 1000-2000°C Draw ratio, carbonization at high temperature for 3 minutes, to prepare carbon fibers with a carbon content of 98.5% and a diameter of 5 μm, and graphitize at a temperature of 2200 ° C, with a residence time of 2.5 minutes, and apply +2% draw ratio to obta...

Embodiment 2

[0013] Using the 12K PAN copolymer fiber produced by Weihai Kaizhan Fiber Co., Ltd., in the air medium, it adopts six stages of pre-oxidation treatment at 190°C, 210°C, 225°C, 235°C, 250°C, and 260°C to obtain a density of 1.34g / cm 3 The preoxidized fiber, other process parameters and operation are the same as embodiment 1, obtains graphite fiber, and the results are shown in Table 1.

Embodiment 3

[0015] The 12K PAN copolymer fiber produced by Weihai Kaizhan Fiber Co., Ltd. is used in six stages of pre-oxidation treatment at 190°C, 210°C, 230°C, 245°C, 255°C, and 265°C in air medium to obtain a density of 1.36g / cm 3 The preoxidized fiber, other process parameters and operation are the same as embodiment 1, obtains graphite fiber, and the results are shown in Table 1.

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Abstract

The invention relates to the field of organic polymer, in particular to a method for preparing high-intensity high-modulus graphite fibers. The method is characterized by comprising the following steps: carrying out pre-oxidation on polyacrylonitrile copolymer fibers in the air atmosphere at a temperature interval of 180 to 280 DEG C; carrying out thermal treatment for 60 to 110min in a 6-stage gradient temperature rising mode to prepare pre-oxidized fibers with density of 1.34 plus and minus 0.02g / cm<3>; carrying out low-temperature carbonization for 3 plus and minus 1.5min under the conventional carbonization conditions, i.e. under the nitrogen protection, a draw ratio is 0 to 4 percent and a temperature is 300 to 900 DEG C; carrying out high-temperature carbonization on the obtained fibers for 3 plus and minus 1.5min at a temperature of 1,000 to 2,000 DEG C under a draw ratio of minus 4 to 0 percent so as to prepare carbon fibers with carbon content of over 98 percent and a diameter of 5mum; carrying out graphitization on the obtained carbon fibers for 2 plus and minus 1min under the protection of inert gas at a temperature of 2,200 to 2,500 DEG C under a draw ratio of 1 to 5 percent so as to obtain the graphite fibers.

Description

technical field [0001] The invention relates to the technical field of carbon fibers, in particular to a method for preparing high-strength and high-modulus graphite fibers. Background technique [0002] We know that carbon fibers can be graphitized at a high temperature of 2200-3000°C to obtain high-modulus graphite fibers with a carbon content of more than 99%. Graphite fibers have excellent properties such as small thermal expansion coefficient, good thermal stability, and stable size. Therefore, It is used to manufacture rigid, thin and dimensionally stable composite components, and is widely used in the fields of spacecraft and aerospace. [0003] In the process of graphitization, the remaining non-carbon elements in the carbon fiber are further removed, the number of network plane rings of the six-membered ring increases, and the graphite crystallites not only grow up, but also align along the fiber axis, so that the interlayer spacing is gradually reduced, and the s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/22D01F11/10
Inventor 张月义王文义丛宗杰李松峰曹明海王宝铭王壮志
Owner WEIHAI TUOZHAN FIBER
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