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Porous Si-B-N-O ultra-fine fiber preparation method

A technology of ultra-fine fibers and fibrils, which is applied in the chemical characteristics of fibers, textiles and papermaking, and rayon of inorganic raw materials, which can solve the problems of poor consistency and poor operability of manual storage of rope nets.

Active Publication Date: 2017-01-18
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a preparation method of porous Si-B-N-O ultrafine fibers, which solves the technical problems of poor consistency and poor operability of the existing rope net manual storage

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0034] This embodiment prepares the preparation method of porous Si-B-N-O ultrafine fiber, comprises the following steps:

[0035] (1) Preparation of spinning solution: polyethylene oxide (M w =1300000), ethanol, dilute acid (1mol / L, dilute hydrochloric acid) were mixed and stirred for 4 hours according to the mass ratio (1:40:20), ultrasonically dispersed into a PEO solution, and the raw materials boric acid, ethyl orthosilicate, vinyl Trimethoxysilane was added to the PEO solution and stirred for 1 hour; wherein the mass ratio of boric acid to ethanol was 0.3:1, the mass ratio of ethyl orthosilicate to ethanol was 2:1, and the mass ratio of vinyltrimethoxysilane to ethanol was The mass ratio is 2:1;

[0036] (2) Electrospinning: use a needle with an inner diameter of 0.8mm, select a voltage of 15kV, a collection distance (vertical distance from the needle tip to the receiving screen) of 12cm, and a feed rate of 15μl / min, the spinning temperature is 20°C, and the relative hu...

Embodiment 2

[0042] The preparation method of the porous Si-B-N-O ultrafine fiber of the present embodiment comprises the following steps:

[0043] (1) Preparation of spinning solution: polyethylene oxide (M w =1300000), ethanol, dilute hydrochloric acid (1mol / L) were mixed and stirred for 4 hours according to the mass ratio (1:40:20), ultrasonically dispersed into a PEO solution, and the raw materials boric acid, methyl orthosilicate, methyl trimethoxy Silane was added to the PEO solution and stirred for 1 hour; the mass ratio of boric acid to ethanol was 0.3:1, the mass ratio of methyl orthosilicate to ethanol was 2:1, and the mass ratio of methyltrimethoxysilane to ethanol was 2 :1;

[0044] (2) Electrospinning: use a needle with an inner diameter of 0.8mm, select a voltage of 15kV, a collection distance of 12cm, and a feed rate of 15μl / min, the spinning temperature is 20°C, and the relative air humidity is 60RH%, and a flat aluminum foil is used for collection Electrospinning the spi...

Embodiment 3

[0049] The preparation method of the Si-B-N-O superfine fiber of the present embodiment, comprises the following steps:

[0050] (1) Preparation of spinning solution: polyethylene oxide (K w =1300000), ethanol, dilute hydrochloric acid (1mol / L) were mixed and stirred for 4 hours according to the mass ratio (1:40:20), ultrasonically dispersed into a PEO solution, and the raw materials boric acid, ethyl orthosilicate, vinyltrimethoxysilane Add it into the PEO solution and stir for 1 hour; the mass ratio of boric acid to ethanol is 0.3:1, the mass ratio of tetraethylorthosilicate to ethanol is 2:1, and the mass ratio of vinyltrimethoxysilane to ethanol is 2:1 ;

[0051] (2) Electrospinning: use a needle with an inner diameter of 0.8mm, select a voltage of 15kV, a collection distance (vertical distance from the needle tip to the receiving screen) of 12cm, and a feed rate of 15μl / min, the spinning temperature is 20°C, and the relative humidity of the air 60RH%, the spinning solut...

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Abstract

A porous Si-B-N-O ultra-fine fiber preparation method includes the steps that 1, a micromolecular boron source, siloxane and modified siloxane serve as solutes, dilute acid and alcohol serve as solvents, a spinning additive is added to prepare a spinning solution, and electrostatic spinning is performed to prepare PBSO (polyborosiloxane) fibrils; 2, the fibrils are put in a drying oven for processing before drying, the dried fibrils are put in a high-temperature furnace in in the atmosphere of NH3 and / or N2 mixed gas for high temperature firing, and porous Si-B-N-O ultra-fine fibers with the diameter of 0.5-5 microns are obtained after the room temperature is reached after cooling. The prepared porous Si-B-N-O ultra-fine fibers are in shapes of fiber felt, are uniform in diameter and have uniform pores internally, the residual carbon content inside the material is low, and the pore range is 2-50 nm. The porous Si-B-N-O ultra-fine fibers have excellent dielectric properties and high temperature resistant performance and have the wide application prospect in aerospace.

Description

technical field [0001] The invention relates to the technical field of high-temperature-resistant wave-transmitting ultrafine ceramic fibers, in particular to a method for preparing porous Si-B-N-O ultrafine fibers. Background technique [0002] Si-B-N-O ceramic fiber felt has the advantages of good high temperature resistance, low thermal conductivity, excellent wave transmission performance, light weight and good flexibility, etc. It has broad application prospects in aviation, aerospace and other fields. [0003] At present, although there are reports on Si-B-N-O ceramics or fibers with large diameters, there are no reports on porous Si-B-N-O ultrafine fibers with uniform diameter distribution. [0004] U.S. Patent US006180809B1 (Patent No. US6180809B1) reported the preparation of polyborosiloxane precursors under an inert protective atmosphere. The precursors were pyrolytically nitridated under ammonia gas at no higher than 1300°C to obtain amorphous Si- B-N-O. The raw...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/10D01F9/08
CPCD01F9/08D01F9/10
Inventor 王应德王兵谢松苏威企
Owner NAT UNIV OF DEFENSE TECH
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