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A kind of core-shell ceramic microsphere and preparation method thereof

A technology of ceramic microspheres and microspheres, applied in the field of SiO2/SiCN core-shell ceramic microspheres and their preparation

Active Publication Date: 2019-05-21
TIANJIN CHENGJIAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current research is mostly based on ZrO 2 and TiO 2 Equal oxide coated SiO 2 Mainly, using the precursor conversion method in SiO 2 The surface coating of non-oxide ceramics to form core-shell structure ceramic microspheres has not been reported

Method used

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  • A kind of core-shell ceramic microsphere and preparation method thereof
  • A kind of core-shell ceramic microsphere and preparation method thereof
  • A kind of core-shell ceramic microsphere and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Add 0.5 g of silicon dioxide and 5 mL of absolute ethanol into the three-necked flask, and put it into an ultrasonic instrument for sufficient ultrasonic dispersion for 15 minutes. Add 0.5 mL of silane coupling agent MPS, and react in a water bath at 40° C. for 24 h. Centrifugal washing, drying. Disperse the modified silica in an aqueous phase system containing 0.1 g of emulsifier OP-100, 7.5 g of deionized water, and 7.5 g of acetonitrile, and add 1 g of polysilazane dropwise to the above aqueous phase system. 0.01ml per minute, ultrasonically dispersed to obtain a uniform emulsion, cross-linked and solidified in an autoclave at 160°C for 4 hours, after the reaction, it was centrifuged and washed three times, dried at 80°C, and then placed in a vacuum furnace for sintering. From room temperature 20 degrees Celsius, the temperature is raised to 1000 degrees Celsius at a rate of 5 degrees Celsius per minute and kept for 5 hours and then cooled to room temperature 20 deg...

Embodiment 2

[0037] Add 0.5 g of silicon dioxide and 5 mL of absolute ethanol into the three-necked flask, and put it into an ultrasonic instrument for sufficient ultrasonic dispersion for 15 minutes. Add 0.5 mL of silane coupling agent MPS, and react in a water bath at 40° C. for 24 h. Centrifugal washing, drying. Disperse the modified silicon dioxide in an aqueous phase system containing 0.2 g of emulsifier OP-100, 15 g of deionized water, and 15 g of acetonitrile, and add 2 g of polysilazane dropwise to the above aqueous phase system at a rate of Minute 0.05ml, ultrasonic dispersion to obtain a homogeneous emulsion, cross-linked and solidified in an autoclave at 200 ° C for 4 hours, after the reaction, it was centrifuged and washed three times, dried at 80 ° C, placed in a vacuum furnace for sintering, from room temperature Start at 25 degrees Celsius and heat up to 1600 degrees Celsius at a rate of 2 degrees Celsius per minute and keep it warm for 1 hour and then cool to room temperat...

Embodiment 3

[0039] Add 0.5 g of silicon dioxide and 5 mL of absolute ethanol into the three-necked flask, and put it into an ultrasonic instrument for sufficient ultrasonic dispersion for 15 minutes. Add 0.5 mL of silane coupling agent MPS, and react in a water bath at 40° C. for 24 h. Centrifugal washing, drying. Disperse the modified silicon dioxide in an aqueous phase system containing 0.2 g of emulsifier OP-10, 15 g of deionized water, and 15 g of acetonitrile, and add 2 g of polysilazane dropwise to the above aqueous phase system at a rate of 0.03ml per minute, ultrasonic dispersion to obtain a homogeneous emulsion, cross-linked and solidified in an autoclave at 200°C for 6 hours, after the reaction, it was centrifuged and washed three times, dried at 80°C, and then placed in a vacuum furnace for sintering. At room temperature of 20 degrees Celsius, the temperature is raised to 1200 degrees Celsius at a rate of 4 degrees Celsius per minute and kept for 3 hours, then cooled to room t...

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Abstract

The invention discloses core-shell ceramic microspheres and a preparation method thereof, and belongs to the technical field of ceramic microspheres; a method combining an emulsion technique and a precursor transformation method is adopted for preparation. The preparation method comprises the steps: firstly, carrying out surface modification of SiO2 with a silane coupling agent, dispersing the modified SiO2 in an aqueous phase system by the emulsion method, dropping an oil phase ceramic precursor polysiloxane, carrying out ultrasonic dispersion to obtain a uniform emulsion, and carrying out a hydrothermal reaction in a high-pressure kettle to obtain SiO2 / PSN microspheres; and then sintering the microspheres in a vacuum furnace, cracking polysilazane at high temperature to form a SiCN ceramic, and thus obtaining the SiO2 / SiCN core-shell ceramic microspheres. The preparation method is simple and has excellent performance; the surface of the SiO2 microspheres is coated with a layer of non-oxidized SiCN shell, and thus the high-temperature heat-insulation performance of the SiO2 based core-shell structure microspheres can be improved.

Description

technical field [0001] The invention belongs to the technical field of ceramic microspheres, in particular to a SiO 2 / SiCN core-shell ceramic microspheres and a preparation method thereof. Background technique [0002] Silica has the characteristics of high purity, low density, large specific surface area, good dispersion performance, and superior thermal stability, chemical inertness, optical and mechanical properties, and is widely used in ceramics, rubber, plastics, coatings, catalyst carriers and Insulation and other fields. However, as a high-temperature insulation material, when the temperature exceeds 800 ° C, SiO 2 Particles are almost transparent to infrared thermal radiation in the 0.75-8 μm band, making it difficult to prevent thermal radiation as a heat transfer method, which limits its application in high-temperature environments. [0003] In order to improve its high-temperature thermal insulation performance, silica-based core-shell structural materials ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/14C04B35/515C04B35/622
Inventor 刘洪丽张海媛杨爱武李婧李亚静李洪彦褚鹏
Owner TIANJIN CHENGJIAN UNIV
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