Preparation method for gradient change silicon-nitrogen-carbon ceramic fibers

A technology of silicon nitrogen carbon ceramics and gradient change, which is applied to the chemical characteristics of fibers, textiles and papermaking, etc. It can solve problems such as difficult to meet the use requirements, and achieve the effects of novel fiber structure, controllability, and simple operation process

Inactive Publication Date: 2017-06-13
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, carbon fiber begins to oxidize in an oxidizing atmosphere of 400°C, and it is difficult to ...

Method used

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  • Preparation method for gradient change silicon-nitrogen-carbon ceramic fibers
  • Preparation method for gradient change silicon-nitrogen-carbon ceramic fibers
  • Preparation method for gradient change silicon-nitrogen-carbon ceramic fibers

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Experimental program
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Effect test

Embodiment 1

[0024] 1) Non-melting treatment: use polymer solid polycarbosilane as a precursor for melt spinning, and then irradiate the precursor with electron beams for crosslinking;

[0025] 2) Nitriding treatment: Put the cross-linked wire obtained in step 1) into a tube furnace, pump and exchange air three times, and pass NH 3 , 1°C / min heating up to 450°C;

[0026] 3) High temperature pyrolysis: Step 2) NH 3 Change to N 2 , the temperature was raised to 1000°C at a heating rate of 2°C / min, kept at a temperature of 120min, and the temperature was lowered to room temperature by program, that is, the gradient silicon nitride / silicon carbide fiber was prepared.

Embodiment 2

[0028] 1) Non-melting treatment: Polymer solid polycarbosilane is used as a precursor for melt spinning, and then the precursor is crosslinked with hot air;

[0029] 2) Nitriding treatment: Put the cross-linked wire obtained in step 1) into a tube furnace, pump and exchange air three times, and pass NH 3 , 3°C / min heating up to 550°C;

[0030] 3) High temperature pyrolysis: Step 2) NH 3 Change to N 2 , the temperature was raised to 1200°C at a heating rate of 5°C / min, kept at a temperature of 60 minutes, and the temperature was lowered to room temperature by program, that is, the gradient silicon nitride / silicon carbide fiber was prepared.

Embodiment 3

[0032] 1) Non-melting treatment: using ultra-high molecular weight solid polycarbosilane as a precursor, melt-spinning to obtain precursors, and then high-temperature thermochemical self-crosslinking to obtain crosslinked fibers;

[0033] 2) Nitriding treatment: Put the cross-linked wire obtained in step 1) into a tube furnace, pump and exchange air three times, and pass NH 3 , 5°C / min to heat up to 650°C;

[0034] 3) High temperature pyrolysis: Step 2) NH 3 Change to N 2 , the temperature was raised to 1400°C at a heating rate of 8°C / min, kept at a temperature of 30min, and then the temperature was lowered to room temperature by program, that is, the gradient silicon nitride / silicon carbide fiber was prepared.

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Abstract

The invention discloses a preparation method for gradient change silicon-nitrogen-carbon ceramic fibers, and relates to an inorganic non-metal material. The preparation method comprises the following steps: performing melt spinning on high-molecular solid-state polycarbosilane serving as a precursor, and then performing non-melting treatment to obtain cross-linking yarns; performing an ammonolysis reaction on the obtained cross-linking yarns under an NH3 atmosphere, and continually pyrolyzing under an N2 atmosphere after reaching a target temperature to obtain the gradient change silicon-nitrogen-carbon ceramic fibers. The high-molecular solid-state polycarbosilane is taken as the precursor which is subjected to the procedures of melt spinning, non-melting treatment, ammoniation, high-temperature pyrolysis and the like to obtain silicon nitride/silicon carbide fibers, and the gradient change of the nitrogen content is regulated and controlled by controlling the ammonolysis temperature. The process is simple, and the operation process is simple and convenient; the controllability of the fiber surface gradient thickness is realized by controlling the ammoniation temperature; the fiber structure is novel, and the fibers have potential application on the aspect of wave absorbing.

Description

technical field [0001] The invention relates to inorganic non-metallic materials, in particular to a method for preparing gradient silicon-nitrogen-carbon ceramic fibers. Background technique [0002] Structural wave-absorbing composite materials reinforced with continuous wave-absorbing fibers have the characteristics of high temperature resistance, light weight, high strength, and high modulus, and also have the function of absorbing electromagnetic waves, which is an important development direction of high-temperature stealth light-weight materials. For example, carbon fiber reinforced resin-based wave-absorbing composite materials have a significant attenuation effect on infrared signals and radar signals, and have excellent chemical stability and mechanical properties. American F-117A, B-2, YF-22, F-22 and advanced cruise missiles, etc. This composite material is widely used (Liang Chunhua. Application of fiber-reinforced ceramic matrix composites in foreign aero-engine...

Claims

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Application Information

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IPC IPC(8): D01F9/10C04B35/584C04B35/565C04B35/622
CPCC04B35/571C04B35/62295D01F9/10
Inventor 刘安华刘星煜苏智明胡志明吴鹏飞于恺瑞唐学原
Owner XIAMEN UNIV
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