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High-temperature resistant micropore silicon carbide fiber and preparation method thereof

A technology of microporous silicon carbide and high temperature resistance, which is applied in the fields of fiber chemical characteristics, melt spinning, chemical post-treatment of rayon, etc. It can solve the problems of poor pore structure stability and low crystallinity, and achieve high temperature resistance. The effect of applying value

Inactive Publication Date: 2011-11-16
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the specific surface area is greatly improved compared with the aforementioned silicon carbide fiber material obtained purely by the cracking of organosilicon polymers, because the fiber still contains 10-20wt% O, and the crystallinity is very low, it is in an amorphous state. The stability of the pore structure is poor, and when used above 900 °C, the specific surface area drops rapidly to 300 m 2 Below / g, not suitable for use under high temperature conditions

Method used

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  • High-temperature resistant micropore silicon carbide fiber and preparation method thereof
  • High-temperature resistant micropore silicon carbide fiber and preparation method thereof
  • High-temperature resistant micropore silicon carbide fiber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The Si content of the microporous silicon carbide fiber in this embodiment is 69.6wt%, the C content is 30.2wt%, the Si:C atomic ratio is 0.99, and the O content is 0.2wt%. 81vol% of the capacity, the specific surface area is 1610m 2 / g, the average pore diameter is 1.72nm. The specific surface area after 10h of use at 1000°C in nitrogen is 1580m 2 / g, the pore structure did not change significantly.

[0023] Preparation: Put 10g of PCS in a melt spinning device, heat it to 280°C under the protection of nitrogen with a purity of 99.999% and perform defoaming treatment, then melt spin at a speed of 100m / min at 240°C and 0.5MPa , to obtain the original silk; put the original silk in the oxidation furnace, heat it to 200 °C at 15 °C / h in the air atmosphere, and keep it warm for 3 hours; use ZnCl to infusible fiber 2 Soak the saturated solution for 20 hours, dry it, place it in a high-temperature furnace protected by nitrogen with a purity of 99.999%, and raise the tempe...

Embodiment 2

[0026] The Si content of the microporous silicon carbide fiber in this example is 69.0wt%, the C content is 30.8wt%, the Si:C atomic ratio is 0.99, and the O content is 0.2wt%. 83vol% of the capacity, the specific surface area is 1034m 2 / g, the average pore diameter is 1.25nm. The specific surface area after 10h of use at 1000°C in nitrogen is 1010m 2 / g, the pore structure did not change significantly.

[0027] Preparation: the only difference from Example 1 is that the activator is H 3 PO 4 .

Embodiment 3

[0029] The Si content of the microporous silicon carbide fiber in this example is 70.1wt%, the C content is 29.8wt%, the Si:C atomic ratio is 1.00, and the O content is 0.1wt%. The capacity is 85vol%, and the specific surface area is 1728m 2 / g, the average pore diameter is 1.76nm. The specific surface area after using in nitrogen at 1000℃ for 10h is 1680m 2 / g, the pore structure did not change significantly.

[0030] Preparation: the only difference from Example 1 is that the activator is ZnCl 2 and H 3 PO 4 mixture.

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Abstract

The invention relates to a high-temperature resistant micropore silicon carbide fiber and a preparation method thereof. The high-temperature resistant micropore SiC fiber is characterized in that: the atomic ratio of Si to C is 0.96 to 1.03, the O content is less than 0.3 weight percent, the fiber has a continuous fiber shape, the micropore volume accounts for over 80vol percent of the total porevolume, the average pore diameter is 1.30 to 2.00 nanometers, and the specific surface area is 1,200 to 2,200 m<2> / g. The preparation method comprises the following steps of: obtaining polycarbosilane infusible fiber by polycarbosilane melting spinning and air non-fusion, cracking the polycarbosilane infusible fiber under the action of activating agent to obtain SiCO fiber, and then performing immersion cleaning on the SiCO fiber by using hydrofluoric acid to obtain the SiC fiber. The SiC fiber of the invention has large specific surface area and good high-temperature resistance, and the porestructure has no obvious change at the temperature of 1,000 DEG C. The SiC fiber has good application prospect in the fields of high-temperature catalysis, gas adsorption and heat insulation.

Description

technical field [0001] The invention relates to a microporous material and a preparation method thereof, in particular to a high temperature resistant microporous silicon carbide fiber and a preparation method thereof. Background technique [0002] Macroporous and mesoporous materials are mainly used as catalyst carriers, filtering macromolecular substances, heat insulation, heat preservation, and sound insulation materials, etc., while microporous materials are mostly used in the fields of adsorption, separation of small molecular substances, and energy storage. Microporous materials are It has been a research hotspot in recent years and has high hopes in the fields of environmental governance, medicine and health, and energy storage. [0003] Inorganic non-metallic microporous materials have become the focus of research due to their good stability, temperature resistance and corrosion resistance. Among them, the most researched microporous materials are mainly carbon mater...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/10D01F11/00D01D1/10D01D5/08D01D10/02
Inventor 楚增勇程海峰王军赫荣安张晓宾王应德李效东
Owner NAT UNIV OF DEFENSE TECH
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