Submicron/nanometer anaerobic silicon carbide fiber felt and preparation method thereof

An oxygen-free silicon carbide, sub-micron technology, applied in fiber processing, fiber chemical characteristics, filament/wire forming, etc., can solve problems affecting fiber high temperature resistance, achieve complete fiber morphology, and improve high temperature resistance Effect

Active Publication Date: 2018-05-04
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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Problems solved by technology

[0005] Aiming at the problem that existing submicron / nanometer SiC fibers contain more oxygen elements, which affect the high temperature resistance of fibers, the main purpose of the present invention is to provide a submicron / nanometer oxygen-free silicon carbide fiber felt and its preparation method to overcome Insufficiency of existing technology

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  • Submicron/nanometer anaerobic silicon carbide fiber felt and preparation method thereof
  • Submicron/nanometer anaerobic silicon carbide fiber felt and preparation method thereof
  • Submicron/nanometer anaerobic silicon carbide fiber felt and preparation method thereof

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preparation example Construction

[0021] One aspect of the embodiments of the present invention provides a method for preparing a submicron / nano-oxygen-free silicon carbide fiber mat, which includes:

[0022] Provide high molecular weight polycarbosilane, the M of the high molecular weight polycarbosilane w Greater than 8000, it does not melt during the process of heating from room temperature to 1000 °C;

[0023] providing a spinning solution containing the homogeneously mixed high molecular weight polycarbosilane, a spinning-assisting polymer and an organic solvent, and performing electrospinning with the spinning solution to obtain a precursor fiber mat;

[0024] In a protective atmosphere, the precursor fiber mat is heated and pyrolyzed to obtain a submicron / nanometer oxygen-free silicon carbide fiber mat.

[0025] As one of the preferred embodiments, the preparation method includes: removing low-molecular-weight polycarbosilane in polycarbosilane with a non-good solvent for polycarbosilane to obtain the ...

Embodiment 1

[0058] (1) Pour PDMS into an autoclave, react at 470°C for 4 hours, add xylene to dissolve the product, filter out the insoluble matter, and evaporate the xylene to obtain T s ≈250~262℃, M w = PCS-1 of 4650. Wrap PCS-1 with filter paper, put it into a Soxhlet extractor, and extract it with acetone 20 times. Rinse the insoluble matter in the filter paper three times with acetone, put it into an oven and dry it under vacuum at 50°C to obtain the M of HPCS-1. w for 8000.

[0059] (2) Under the condition of magnetic stirring, dissolve HPCS-1 and PS in the mixed organic solvent of xylene and dimethylformamide, stir well until a transparent and clear solution is formed, which is the spinning solution. Among them, the mass ratio of HPCS-1:PS:organic solvent is 30:5:65.

[0060] (3) Put the spinning solution obtained above into the electrospinning device, the diameter of the spinneret is 1.0 mm, the set output voltage is 14 kV, the feeding rate is 20 μl / min, the distance of the sp...

Embodiment 2

[0064] (1) Pour PDMS into an autoclave, react at 480°C for 2 hours, add xylene to dissolve the product, filter out the insoluble matter, and evaporate the xylene to obtain T s ≈267~283℃, M w = PCS-2 of 4760. Wrap PCS-2 with filter paper, put it into a Soxhlet extractor, and extract it with isopropanol 10 times. Rinse the insoluble matter in the filter paper three times with isopropanol, put it in an oven and dry it under vacuum at 70°C to obtain the M of HPCS-2. w for 9970.

[0065] (2) Under the condition of magnetic stirring, dissolve HPCS-2 and PEO in a mixed organic solvent of xylene and acetone, and stir well until a transparent and clear solution is formed, which is the spinning solution. Among them, the mass ratio of HPCS-2:PEO:organic solvent is 12:3:85.

[0066] (3) Put the spinning solution obtained above into the electrospinning device, the diameter of the spinneret is 1.2mm, the set output voltage is 20kV, the feeding rate is 10μl / min, the distance of the spinn...

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Abstract

The invention discloses submicron / nanometer anaerobic silicon carbide fiber felt and a preparation method thereof. The preparation method includes the steps of providing a spinning solution containinghigh-molecular-weight polycarbosilane with the Mw greater than 8000, a spinning-assisting polymer and an organic solvent which are uniformly mixed, performing electrospinning with the spinning solution to obtain precursor fiber felt, and performing heating pyrolysis treatment on the precursor fiber felt in a protective atmosphere to obtain the submicron / nanometer anaerobic silicon carbide fiber felt. According to the preparation method, soluble and infusible high-molecular-weight polycarbosilane is adopted to prepare the submicron / nanometer anaerobic silicon carbide fiber felt, and as high-molecular-weight polycarbosilane does not need air infusibility treatment in the heating process, it is avoided that oxygen is introduced into the submicron / nanometer anaerobic silicon carbide fiber felt; besides, after the silicon carbide fiber felt is treated at the temperature reaching 1600 DEG C in an inert atmosphere, the mass decrement is smaller than 2wt%, and the complete fiber morphology can still be maintained.

Description

technical field [0001] The invention relates to a method for preparing a silicon carbide fiber felt, in particular to a method for preparing a submicron / nano oxygen-free silicon carbide fiber felt by using high molecular weight polycarbosilane, and belongs to the technical field of preparing ceramic fibers by a precursor method. Background technique [0002] SiC has excellent properties such as high temperature resistance, oxidation resistance, and corrosion resistance. The components prepared from it have broad application prospects in harsh environments such as high temperature, strong corrosion, and neutron irradiation. Professor Yajima of Japan prepared SiC fibers with a diameter of 10-20 μm by the precursor method, that is, using polycarbosilane (hereinafter also referred to as PCS) as the precursor, and preparing SiC fibers by melt spinning, non-melting treatment and high temperature pyrolysis . [0003] Electrospinning technology is an effective method that can direc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D04H1/728D01D5/00D01F6/94
CPCD01D5/003D01F6/94D04H1/728
Inventor 袁钦黄庆顾喜双
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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