Silicon carbide fibers having a low oxygen content and a preparing method thereof

A silicon carbide fiber and fiber technology, which is applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of the decline of SiC fiber performance, and achieve the effect of improving mechanical properties and high temperature resistance, good high temperature resistance and good mechanical properties.

Active Publication Date: 2018-05-15
江西信达航科新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, in the non-melting process of the precursor conversion method, if the economical air crosslinking method is used, it is easy to introduce a large amount of oxygen; due to the large amount of oxygen in the SiC fiber x o y The amorphous state of SiC fiber exists, and it is easy to undergo thermal decomposition at high temperature, which makes the performance of SiC fiber drop sharply at high temperature.

Method used

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  • Silicon carbide fibers having a low oxygen content and a preparing method thereof

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preparation example Construction

[0026] The invention provides a method for preparing silicon carbide fibers with low oxygen content, comprising the following steps:

[0027] S100: Purification of raw materials

[0028] Polycarbosilane (PCS) was synthesized from polydimethylsilane (PDMS) with a molecular weight of 2500-3000, and the liquid low-molecular by-product polysilicon carbon with a softening point of 180-200°C and a number-average molecular weight of 1600-2200 was collected. Silane (PSCS); PSCS is then dissolved in an appropriate amount of xylene solvent, filtered, and distilled under reduced pressure to obtain the pure product PSCS. Wherein, the volume ratio of xylene to by-product polysilocarbosilane is (1-2):1.

[0029] S101: Preparation of polyaluminocarbosilane (PACS) precursor

[0030] Take the aluminum acetylacetonate (Al(AcAc) which is 5-10% by mass percent 3 ) placed in the autoclave, the pure product PSCS was slowly injected into the autoclave, evenly covered in Al(AcAc) 3 surface; then ...

Embodiment 1

[0040] The invention provides a method for preparing silicon carbide fibers with low oxygen content, comprising the following steps:

[0041] S100: Purification of raw materials

[0042] Synthesize polycarbosilane (PCS) with polydimethylsilane (PDMS) as raw material, collect liquid low molecular by-product polysilocarbosilane (PSCS); then dissolve PSCS in an appropriate amount of xylene solvent, filter, and distill under reduced pressure , to obtain the pure product PSCS. Wherein, the volume ratio of xylene to by-product polysilocarbosilane is 1:1.

[0043] S101: Preparation of polyaluminocarbosilane (PACS) precursor

[0044] Get mass percent concentration and be 10% aluminum acetylacetonate (Al(AcAc) 3 ) placed in the autoclave, the pure product PSCS was slowly injected into the autoclave, evenly covered in Al(AcAc) 3 surface; then pass through N 2 permutation 3 times, followed by N 2 Slowly heat to 360°C at a rate of 5°C / min under the atmosphere, and keep it warm for 6...

Embodiment 2

[0052] The invention provides a method for preparing silicon carbide fibers with low oxygen content, comprising the following steps:

[0053] S100: Purification of raw materials

[0054] Synthesize polycarbosilane (PCS) with polydimethylsilane (PDMS) as raw material, collect liquid low molecular by-product polysilocarbosilane (PSCS); then dissolve PSCS in an appropriate amount of xylene solvent, filter, and distill under reduced pressure , to obtain the pure product PSCS. Wherein, the volume ratio of xylene to by-product polysilocarbosilane is 2:1.

[0055] S101: Preparation of polyaluminocarbosilane (PACS) precursor

[0056] Get mass percent concentration and be 5% aluminum acetylacetonate (Al(AcAc) 3 ) placed in the autoclave, the pure product PSCS was slowly injected into the autoclave, evenly covered in Al(AcAc) 3 surface; then pass through N 2 permutation 3 times, followed by N 2 Slowly heat to 400°C at a rate of 10°C / min under the atmosphere, and keep it warm for 5...

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Abstract

The invention relates to silicon carbide fibers having a low oxygen content and a preparing method thereof. The method includes S101) reacting aluminum acetylacetonate with polysilacarbosilane to obtain a polyaluminocarbosilane crude material, dissolving the crude material with xylene, and performing filtration and vacuum distillation to obtain a refined polyaluminocarbosilane material; S102) subjecting the refined material to melting spinning treatment to obtain a polyaluminocarbosilane fiber bundle; S103) then performing curing treatment with air to obtain crosslinked fibers; and S104) sintering the crosslinked fibers at a high temperature in an inert atmosphere to obtain the silicon carbide fibers. The prepared silicon carbide fibers have excellent mechanical performance and high-temperature resistance. At room temperature, strength of the silicon carbide fibers can be 2.8 + / - 0.3 GPa, and elasticity modulus is 210 + / - 10 GPa. After the silicon carbide fibers are treated at 1000 DEGC in an air atmosphere for 100 h, the strength retention rate can be still 80% or above, and therefore the silicon carbide fibers have wide application value and a wide application prospect in the field of high-performance fibers.

Description

technical field [0001] The invention relates to the technical field of high-performance fibers, in particular to a silicon carbide fiber with low oxygen content and a preparation method thereof. Background technique [0002] Silicon carbide (SiC) fiber, as a high-strength, high-modulus ceramic fiber with excellent high-temperature oxidation resistance, has extremely broad application prospects in high-tech fields such as aviation, aerospace, and weapons. Specifically, SiC fibers have high strength and good weaving performance, and can be applied to different polymer-based, metal-based, and ceramic-based composite materials through different interface treatments. [0003] Due to the excellent properties of SiC fibers, countries around the world have carried out extensive research on the preparation of continuous SiC fibers. At present, the main methods for preparing continuous SiC fibers are: chemical vapor deposition method (CVD method), chemical vapor phase reaction method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/10
CPCD01F9/10
Inventor 吴宝林侯振华
Owner 江西信达航科新材料科技有限公司
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