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A kind of ultra-long silicon nitride/silica core-shell structure nanofiber and its preparation method

A technology of silica and core-shell structure, applied in the direction of fiber chemical characteristics, conjugated artificial filaments, artificial filaments made of inorganic materials, etc., can solve the problem of increasing the overall cost of silicon nitride nanofibers, increasing process complexity and difficulty, The cost of rare earth metal salts is high, and the preparation process is simple and easy to implement, the preparation method is simple and efficient, and the effect is relatively easy to obtain

Active Publication Date: 2022-06-28
苏州纤创智造新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method requires rare earth metal salts as catalysts. Most of the rare earths are distributed on the earth with relatively low concentrations. There are relatively few regions with rich rare earth reserves in the world, which are scarce resources. Therefore, most of the rare earth metal salts are expensive. The preparation method uses rare earth metal salts as catalysts, although it can be reused in theory, but in actual operation, the sparse metal salts need to be extracted again from the waste liquid, which undoubtedly increases the complexity and difficulty of the process, and also increases the preparation of nitriding. The overall cost of silicon nanofibers, and without effective recycling technology, the production method requires repeated consumption of rare earth resources
It can be seen that although the preparation method in the prior art can prepare one-dimensional Si 3 N 4 Nanostructure, but consumes rare earth resources, and the cost is high, this drawback has become an obstacle that cannot be ignored in large-scale production

Method used

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  • A kind of ultra-long silicon nitride/silica core-shell structure nanofiber and its preparation method
  • A kind of ultra-long silicon nitride/silica core-shell structure nanofiber and its preparation method
  • A kind of ultra-long silicon nitride/silica core-shell structure nanofiber and its preparation method

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preparation example Construction

[0030] The preparation method of ultra-long silicon nitride / silicon dioxide core-shell nanofibers provided by the present invention comprises the following steps:

[0031] (1) Preparation of precursor solution: weigh a certain mass of silicon source and add it to the polar solvent, stir and disperse at 20-100 ° C for 1-8 h, and add a certain mass of polymer-based carbon source after fully dispersed, Continue to stir for 4-12h, let stand or defoaming under reduced pressure for later use.

[0032] (2) Precursor molding: the precursor solution obtained in the step (1) is subjected to a casting film method or a spinning method to solidify and shape to obtain a precursor of a highly dispersed silicon source / polymer-based carbon source mixture.

[0033] (3) heat treatment of precursor: put the precursor obtained in the step (2) into a high-temperature furnace, carry out nitridation treatment under nitrogen atmosphere, drop to room temperature after the heat treatment process is comp...

Embodiment 1

[0044] S11: Preparation of precursor solution: 30 g of SiO 2 Nanoparticles (particle size: 7-40 nm) were added to 900 ml of N,N-dimethylformamide solvent, and ultrasonically dispersed for 1 h at room temperature. 70g of polyacrylonitrile (molecular weight M w =50,000), stirred and dispersed at 55°C for 12h to form a homogeneous mixed solution, filtered through an 800-mesh filter for use.

[0045] S12: Precursor forming: pump the precursor solution in step S11 into the metering pump for casting film, extrude the die 1000mm, the mechanical speed is 500m / h, the microscopic morphology of the obtained film-like precursor is shown in figure 1 shown.

[0046] S13: Heat treatment of the precursor: place the film-like precursor in step S12 in a high-temperature furnace, heat it up to 1400°C at a heating rate of 7°C / min in a nitrogen atmosphere, and perform nitridation for 2 hours to obtain ultra-long Silicon nitride / silica core-shell nanofibers, the morphology and structure of which...

Embodiment 2

[0049] The high-temperature nitridation time in step S13 in Example 1 is adjusted to 3h, and the remaining steps are the same as those in Example 1, so that ultra-long silicon nitride / silicon dioxide core-shell nanofibers can be obtained.

[0050] The diameter of the silicon nitride / silicon dioxide core-shell nanofibers obtained in this example is slightly increased, distributed in the range of 80-200 nm, and the aspect ratio is large, greater than 1000.

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Abstract

The invention provides an ultra-long silicon nitride / silicon dioxide core-shell nanofiber and a preparation method thereof, which belong to the technical field of ceramic matrix composite materials. In this method, the silicon source is added to the polar solvent, stirred at 20-100°C for 1-8h, and then the polymer-based carbon source is added, and the precursor solution is obtained after standing still or degassing under reduced pressure; the co-precipitation method is adopted One or more of casting method, spinning method to shape and solidify the precursor solution; then put it into a high-temperature furnace, carry out nitriding treatment in a nitrogen atmosphere, and then lower it to 20-25°C, Take it out to get ultra-long silicon nitride / silicon dioxide core-shell nanofibers. Compared with the prior art, the present invention does not need to consume rare earth metals, nor does it require metal catalysts or templates, the preparation process is simple and efficient, and the prepared silicon nitride / silica core-shell nanofibers have high purity and high yield, and the diameter and The length is controllable, suitable for mass production.

Description

technical field [0001] The invention relates to the technical field of ceramic matrix composite materials, in particular to an ultra-long silicon nitride / silicon dioxide core-shell nanofiber and a preparation method thereof. Background technique [0002] Silicon nitride (Si 3 N 4 ) is an important wide-bandgap high-performance ceramic material with a series of excellent properties such as high temperature resistance, oxidation resistance, high strength, high hardness, impact resistance, wear resistance, strong chemical stability, and good lubricating properties. It is used in the field of high-performance device fabrication and high-temperature resistant semiconductor materials. one-dimensional Si 3 N 4 Nanostructures not only have Si 3 N 4 The basic advantages of bulk materials, but also the unique geometric structure and special physical and chemical properties of one-dimensional nanomaterials. Si 3 N 4 Nanofibers, as the third-generation wide-bandgap (5.3 eV) sem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F8/18D01F9/08
CPCD01F8/18D01F9/08
Inventor 韩春梅李先锋
Owner 苏州纤创智造新材料科技有限公司
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