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Preparation method of flexible porous silicon carbide micro-nano fibrofelt

A technology of micro-nano fiber and porous silicon carbide, which is applied in the directions of fiber treatment, fiber chemical characteristics, spinning solution preparation, etc., can solve the problem of low yield of spinning fiber, the preparation method of flexible porous silicon carbide micro-nano fiber mat, It is not suitable for large-scale preparation and other problems, and achieves the effects of good flexibility, small fiber diameter and high production efficiency

Active Publication Date: 2013-10-09
LVNA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Very dilute solution spinning fiber yield is low, not suitable for large-scale preparation
[0004] At present, there is no relevant report on the preparation method of flexible porous silicon carbide micro-nano fiber mat

Method used

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  • Preparation method of flexible porous silicon carbide micro-nano fibrofelt
  • Preparation method of flexible porous silicon carbide micro-nano fibrofelt
  • Preparation method of flexible porous silicon carbide micro-nano fibrofelt

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Mixed solvents of xylene, tetrahydrofuran and dimethylformamide were prepared at a volume ratio of 3:1:1. 5.0 g of polyaluminocarbosilane was added to 5.0 g of the mixed solvent and fully stirred for 4 hours to obtain a polyaluminocarbosilane solution with a concentration of 50 wt%. Place the solution for 8 days, put it into a glass syringe, the spinneret is 8# metal needle, under the conditions of output voltage 18kV, injection flow rate 2.0mL / h, roller accepting distance 8cm, humidity 40%, room temperature Electrospinning was carried out, and a flexible porous polyaluminocarbosilane fiber felt was obtained after spinning for 3 hours; then, in an air atmosphere, the temperature was raised to 200°C at a heating rate of 10°C / min and kept for 2h for oxidative cross-linking, and finally at 1300°C, high-purity nitrogen After the atmosphere treatment for 1 hour, a flexible porous silicon carbide micro-nano fiber mat is obtained, the fiber diameter is distributed around 1.5 μ...

Embodiment 2

[0024] Prepare a mixed solvent of xylene and dimethylformamide at a volume ratio of 7:3. 6.0 g of polyaluminocarbosilane was added to 4.0 g of the mixed solvent and stirred thoroughly for 6 hours to obtain a polyaluminocarbosilane solution with a concentration of 60 wt%. After placing the solution for 5 days, put it into a glass syringe, the spinneret is 8# metal needle, and carry out electrospinning at room temperature at an output voltage of 20kV, an injection flow rate of 2.0mL / h, a flat aluminum foil collection distance of 10cm, and a humidity of 60%. Silk, after spinning for 3 hours, a flexible porous polyaluminocarbosilane fiber felt was obtained; then, in an air atmosphere, the temperature was raised to 200°C at a heating rate of 15°C / min and kept for 2h for oxidative cross-linking, and finally treated at 1200°C in a high-purity nitrogen atmosphere for 2h , to obtain a flexible porous silicon carbide micro-nano fiber mat.

Embodiment 3

[0026] Prepare a mixed solvent of toluene, acetone and ethanol at a volume ratio of 3:1:1. Weighing 6.5 g of polycarbosilane was added to 3.5 g of mixed solvent and stirred thoroughly for 6 hours to obtain a polycarbosilane solution with a concentration of 65 wt%. After placing the solution for 7 days, put it into a glass syringe, the spinneret is a 12# metal needle, and the output voltage is 25kV, the injection flow rate is 1.5mL / h, the receiving distance of the drum is 12cm, the humidity is 50%, and it is carried out at room temperature. Electrospinning, after spinning for 2.5 hours, a flexible porous polycarbosilane fiber felt was obtained; then, in an air atmosphere, the temperature was raised to 180°C at a heating rate of 10°C / min and kept for 2h for oxidative cross-linking, and finally at 1000°C in a high-purity nitrogen atmosphere After 1 hour of treatment, a flexible porous silicon carbide micro-nano fiber mat is obtained.

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Abstract

The invention provides a preparation method of a flexible porous silicon carbide micro-nano fibrofelt, relating to silicon carbide fibers. The invention provides a preparation method of a flexible porous silicon carbide micro-nano fibrofelt which is small in fiber diameter and enriched in nano-pores and can realize a flexible porous characteristic. The preparation method comprises the following steps of: mixing and uniformly stirring a good solvent and a non-solvent in proportion to obtain a mixed solvent; dissolving a silicon carbide ceramic precursor containing a silicon polymer in the mixed solvent, adding an electrolyte, and stirring until the components are fully dissolved to obtain an electrostatic spinning solution; performing electrostatic spinning on the obtained electrostatic spinning solution through an electrostatic spinning device, and continuously spinning to obtain precursor micro-nano fibrofelts with different thicknesses; and heating the obtained precursor micro-nano fibrofelts, performing drying and oxidation crosslinking, then heating again under the protection of an inert atmosphere, and performing high temperature pyrolysis to obtain the flexible porous silicon carbide micro-nano fibrofelt. The process is simple and high in production efficiency; and the fiber diameter of the obtained fibrofelt is 0.5-3 microns, and the nano-pore diameter is 5-100 nanometers.

Description

technical field [0001] The invention relates to silicon carbide fibers, in particular to a method for preparing a flexible porous silicon carbide micro-nano fiber mat. Background technique [0002] Porous silicon carbide materials have the characteristics of low density, high temperature resistance, corrosion resistance, high temperature resistance, high specific surface area, high permeability, and high mechanical properties. They have broad application prospects in high-temperature filtration, catalyst loading, wave-absorbing stealth, high-temperature sensors, etc. . Especially in special fields, such as in the field of nuclear energy, it is used for high-temperature cold air to filter radioactive waste liquid and high-temperature helium containing graphite particles, and porous silicon carbide materials become ideal materials. At present, porous silicon carbide is mainly block ceramics, which are formed by pressing raw material powder and then sintering at high temperatu...

Claims

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Application Information

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IPC IPC(8): D04H3/002D04H3/16D01D1/02D01D5/00D01F9/10
Inventor 余煜玺陈勇
Owner LVNA TECH CO LTD
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