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Bulk silicon carbide polymer precursor ceramic and blending-cracking preparation method thereof

A precursor and silicon carbide technology, which is applied in the field of bulk silicon carbide polymer precursor ceramics and blending and recracking preparation, can solve the problems of low ceramic yield, large shrinkage rate of single-piece ceramics, and difficulty in forming ceramics. Good hardness and fracture toughness performance, ensuring ceramic structural integrity, practicability and reliability

Active Publication Date: 2019-11-19
中科德胜(常州)电子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the precursor transformation method is relatively mature in the preparation of one-dimensional and two-dimensional silicon carbide materials, and the product performance is good. There are many obstacles such as shrinkage and more free carbon residues, among which the problem of block forming is particularly prominent
Due to the high content of organic groups in the precursor, a large amount of gas will be generated during the cracking process, resulting in defects such as cracks and pores in large-sized monolithic and bulk ceramics, and destroying the integrity of bulk silicon carbide ceramics
The applicant disclosed in Chinese patent CN 108129151 A a method for preparing graphene / silicon carbide nanocomposite structure monolithic ceramics by high-temperature pyrolysis of graphene oxide-vinyltriethoxysilane-polycarbosilane precursor, a breakthrough However, the shrinkage rate of the monolithic ceramics obtained is large, the ceramic yield is low, the fracture toughness is poor, and there are many holes and defects on the microscopic scale, which affect the comprehensive performance of the ceramics.

Method used

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  • Bulk silicon carbide polymer precursor ceramic and blending-cracking preparation method thereof
  • Bulk silicon carbide polymer precursor ceramic and blending-cracking preparation method thereof
  • Bulk silicon carbide polymer precursor ceramic and blending-cracking preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 1. Dissolve 1g of PCS powder with a relative molecular weight of 1426g / mol in 20mL of xylene, add 1mL of VTES and an appropriate amount of Castor catalyst to it, and obtain a golden yellow transparent liquid;

[0030] 2. Disperse 0.01g of GO powder in 20mL of purified water, and then mix it with the xylene solution in step 1;

[0031] 3. Take the mixed solution in step 2 and heat it in a 60°C water bath, and stir the reaction with a magnetic stirrer for 30 minutes. After standing still, take the upper liquid and spin evaporate and grind it to obtain the precursor PVG solid powder;

[0032] 4. Put the precursor PVG powder in a crucible, and crack it in an argon atmosphere with a flow rate of 100mL / min. The cracking temperature is 1200°C, the heating rate is 4°C / min, and the holding time is 1min to obtain cracked SiC(rGO) p ceramic particles;

[0033] 5. Take cracked SiC(rGO) with a mass ratio of 6:4 p Ceramic particles and its precursor PVG powder to obtain SiC(rGO) p...

Embodiment 2

[0038] 1. Dissolve 1g of PCS powder with a relative molecular weight of 1426g / mol in 20mL of xylene, add 1mL of VTES and an appropriate amount of Castel catalyst to it, and obtain a golden yellow transparent liquid;

[0039] 2. Disperse 0.01g of GO powder in 20mL of purified water, and then mix it with the xylene solution in step 1;

[0040] 3. Take the mixed solution in step 2 and heat it in a 60°C water bath, and stir the reaction with a magnetic stirrer for 30 minutes. After standing still, take the upper liquid and spin evaporate and grind it to obtain the precursor PVG solid powder;

[0041] 4. Put the precursor PVG powder in a crucible, and crack it in an argon atmosphere with a flow rate of 100mL / min. The cracking temperature is 1200°C, the heating rate is 4°C / min, and the holding time is 1min to obtain cracked SiC(rGO) p ceramic particles;

[0042] 5. Take cracked SiC(rGO) with a mass ratio of 7:3 p Ceramic particles and its precursor PVG powder to obtain SiC(rGO) p...

Embodiment 3

[0047] 1. Dissolve 1g of PCS powder with a relative molecular weight of 1426g / mol in 20mL of xylene, add 1mL of VTES and an appropriate amount of Castor catalyst to it, and obtain a golden yellow transparent liquid;

[0048] 2. Disperse 0.01g of GO powder in 20mL of purified water, and then mix it with the xylene solution in step 1;

[0049] 3. Take the mixed solution in step 2 and heat it in a 60°C water bath, and stir the reaction with a magnetic stirrer for 30 minutes. After standing still, take the upper liquid and spin evaporate and grind it to obtain the precursor PVG solid powder;

[0050] 4. Put the precursor PVG powder in a crucible, and crack it in an argon atmosphere with a flow rate of 100mL / min. The cracking temperature is 1200°C, the heating rate is 4°C / min, and the holding time is 1min to obtain cracked SiC(rGO) p ceramic particles;

[0051] 5. Take cracked SiC(rGO) with a mass ratio of 8:2 p Ceramic particles and its precursor PVG powder to obtain SiC(rGO) p...

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Abstract

The invention provides a bulk silicon carbide polymer precursor ceramic and a blending-cracking preparation method thereof, belonging to the field of preparation of ceramic materials. The bulk siliconcarbide polymer precursor ceramic is named as 3D-SiC(rGO) ceramic and is composed of beta-SiC, SiO<x>C<y>, SiO<2>, rGO, and free carbon, wherein beta-SiC nanocrystals are dispersed in a SiO<x>C<y> / C<free> amorphous phase, and SiO2 grains are inlaid in a beta-SiC / SiO<x>C<y> / C<free> matrix. The homemade modified polymer precursor polycarbosilane-vinyltriethoxysilane-graphene oxide is used as a rawmaterial and is mixed with SiC(rGO) powder obtained after cracking the precursor in proportion, and then ball milling and re-cracking are carried out so as to prepare the ceramic. The ceramic has high ceramic yield, low linear shrinkage, good hardness and fracture toughness, uniform and dense microstructure, few pores, microcracks and interfaces, and good practicality and reliability.

Description

technical field [0001] The invention relates to the preparation of ceramic materials, in particular to a bulk silicon carbide polymer precursor ceramic and a preparation method of blending and cracking. Background technique [0002] As an advanced structural ceramic material, silicon carbide ceramics have outstanding characteristics such as high hardness, corrosion resistance, wear resistance, good thermal conductivity, and stable chemical properties. They can work normally under harsh conditions such as high temperature, high power, and high frequency. Applied in industrial production, it has broad development prospects in the fields of energy, electronics, chemical industry, national defense, metallurgy, aerospace and other fields. [0003] The traditional preparation methods of bulk silicon carbide ceramics include pressureless sintering, hot pressing sintering, hot isostatic pressing sintering, reaction sintering and so on. Chinese patent ZL 201810338310.2 discloses a p...

Claims

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Application Information

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IPC IPC(8): C04B35/571C04B35/577C04B35/622
CPCC04B35/571C04B35/622C04B2235/3418C04B2235/3895C04B2235/424C04B2235/425C04B2235/483C04B2235/656C04B2235/6567C04B2235/658C04B2235/9615
Inventor 姚荣迁郑艺浓林舒宇廖亮韩宇宸钟磊钟跃进李凌杰庄堃黄雯燕
Owner 中科德胜(常州)电子科技有限公司
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