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Submicron silicon nitride hollow microspheres and preparation method

A submicron silicon nitride technology, which is applied in the field of submicron silicon nitride hollow microspheres and its preparation, can solve the problems of large particle size and uneven particle size of silicon nitride hollow microspheres, and achieve uniform particle size, Low cost, uniform and controllable effect

Active Publication Date: 2019-08-02
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to avoid the deficiencies of the prior art, the present invention proposes a submicron silicon nitride hollow microsphere and its preparation method, which solves the problem of large particle size and uneven particle size of the silicon nitride hollow microsphere prepared in the prior art. technical issues

Method used

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  • Submicron silicon nitride hollow microspheres and preparation method

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Embodiment 1

[0038] Step 1. Preparation of monodisperse SiO by modified Stober method 2 Microspheres

[0039] Step 1.1, mix 24ml of deionized water, 100ml of absolute ethanol and 14ml of concentrated ammonia water, then stir at 30°C for 20min, and obtain solution A after stirring.

[0040] Step 1.2, suck 6ml tetraethyl orthosilicate into the syringe, add it dropwise into solution A at a rate of 3.75ml / h, stir at 30°C for 12h, collect the final solution by centrifugation and wash it three times with absolute ethanol. Insulate in an oven at 80°C for 24 hours to obtain monodisperse SiO 2 Microspheres.

[0041] Step 2. Preparation of phenolic resin-coated silica core-shell powder SiO by polycondensation reaction of resorcinol and formaldehyde 2 @RF(Resorcinol-formaldehyde resin)

[0042] The monodisperse SiO prepared in step 1 2Put the microspheres into the Erlenmeyer flask, add a mixed solution of distilled water and absolute ethanol, then add concentrated ammonia water, cetyltrimethylam...

Embodiment 2

[0051] Step 1. Preparation of monodisperse SiO by modified Stober method 2 Microspheres

[0052] Step 1.1, mix 24ml of deionized water, 100ml of absolute ethanol and 14ml of concentrated ammonia water, then stir at 30°C for 20min, and obtain solution A after stirring.

[0053] Step 1.2, suck 6ml tetraethyl orthosilicate into the syringe, add it dropwise to solution A at a rate of 1ml / h, stir at 30°C for 12h, collect the final solution by centrifugation and wash it three times with absolute ethanol. ℃ in the oven for 24h, that is, monodisperse SiO 2 Microspheres.

[0054] Step 2. Preparation of phenolic resin-coated silica core-shell powder SiO by polycondensation reaction of resorcinol and formaldehyde 2 @RF(Resorcinol-formaldehyde resin)

[0055] The monodisperse SiO prepared in step 1 2 Put the microspheres into the Erlenmeyer flask, add a mixed solution of distilled water and absolute ethanol, then add concentrated ammonia water, cetyltrimethylammonium bromide, and res...

Embodiment 3

[0064] Step 1. Preparation of monodisperse SiO by modified Stober method 2 Microspheres

[0065] Step 1.1, mix 24ml of deionized water, 100ml of absolute ethanol and 14ml of concentrated ammonia water, then stir at 30°C for 20min, and obtain solution A after stirring.

[0066] Step 1.2, suck 6ml tetraethyl orthosilicate into the syringe, add it dropwise into solution A at a rate of 3.75ml / h, stir at 30°C for 12h, collect the final solution by centrifugation and wash it three times with absolute ethanol. Insulate in an oven at 80°C for 24 hours to obtain monodisperse SiO 2 Microspheres.

[0067] Step 2. Preparation of phenolic resin-coated silica core-shell powder SiO by polycondensation reaction of resorcinol and formaldehyde 2 @RF(Resorcinol-formaldehyde resin)

[0068] The monodisperse SiO prepared in step 1 2 Put the microspheres into the Erlenmeyer flask, add a mixed solution of distilled water and absolute ethanol, then add concentrated ammonia water, cetyltrimethyla...

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Abstract

The invention relates to submicron silicon nitride hollow microspheres and a preparation method. The preparation method is technically characterized by comprising steps as follows: (1), silicon dioxide microspheres synthesized with a stober method are taken as a silicon source, phenol-formaldehyde resin synthesized from resorcinol and formaldehyde is taken as a carbon source, and a synthesized SiO2@RF(Resorcinol-formaldehyde resin) core-shell structure is taken as a precursor; (2) a certain quantity of the precursor prepared in step (1) is subjected to a carbothermal reduction-nitridation reaction at a certain temperature; (3), powder prepared in step (2) is oxidized to remove carbon and subjected to acid pickling to remove silicon dioxide, and the silicon nitride hollow microspheres are obtained. With the adoption of the technical scheme, the submicron silicon nitride hollow microspheres with controllable and uniform particle size, uniform microstructure and morphology and relativelypure composition can be prepared. The preparation technology is stable, high in repeatability and low in cost and facilitates mass production of the silicon nitride hollow microspheres.

Description

technical field [0001] The invention belongs to the technical field of preparation of new materials, and relates to a submicron silicon nitride hollow microsphere and a preparation method. Background technique [0002] Silicon nitride ceramics have the characteristics of high strength, high temperature resistance, and corrosion resistance. They are excellent high-temperature structural materials and can be used in hot-end parts in aviation and aerospace fields. However, the dielectric constant of silicon nitride ceramics is relatively high, and the thermal conductivity and density are relatively high. It is difficult to meet the multi-functional requirements of broadband wave transmission, integrated heat insulation, and light weight at the same time, which limits its application in the fields of aviation and aerospace. Wider application. In order to cope with more harsh and complex service environments, it is urgent to develop new silicon nitride ceramics. By designing and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/587C04B35/626
CPCC04B35/587C04B35/62605
Inventor 成来飞赵凯叶昉张立同
Owner NORTHWESTERN POLYTECHNICAL UNIV
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