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Molybdenum disilicide/silicon carbide three-dimensional polymer precursor ceramic and preparation method thereof

A molybdenum disilicide and precursor technology, applied in the field of molybdenum disilicide/silicon carbide three-dimensional polymer precursor ceramics and their preparation, can solve the problems of excessive residual silicon content, ceramic cracks, poor mechanical properties of silicon carbide ceramics, etc. Achieve uniform and dense microstructure, high thermal and electrical conductivity, and good composition uniformity

Active Publication Date: 2020-10-30
中科德胜(常州)电子科技有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

Chinese patent ZL 201610850564.3 discloses a method for preparing silicon carbide ceramic materials with low residual silicon by a multi-step reaction sintering method, mixing different carbon sources into silicon carbide powder, adding phenolic resin or PVA mechanical mixing, and vacuum conditions at 1600-1700 °C High-density silicon carbide ceramics with better thermal conductivity and high-temperature mechanical properties can be obtained by lower sintering, and at the same time, the problem of poor mechanical properties caused by excessive residual silicon content in silicon carbide ceramics is solved
The polycarbosilane precursor escapes a large amount of small molecule gas during cracking, causing a large number of holes in the ceramic to affect the density, or shrinkage causes a large number of cracks in the ceramic, which eventually causes serious damage and cannot be molded, and the amorphous SiOxCy phase and free carbon phase The presence of silicon carbide ceramics makes the mechanical properties poor
Chinese patent ZL 201711494377.7 discloses a method for preparing graphene / silicon carbide monolithic ceramics by high-temperature pyrolysis of graphene oxide-vinyltriethoxysilane-polycarbosilane precursors, and preparing three-dimensional silicon carbide ceramics by the precursor method New breakthroughs have been made in the field, but the overall performance of the obtained monolithic ceramics is not good, which limits its application
Chinese patent CN 110467467 A discloses a method of blending and re-cracking, which makes graphene / silicon carbide monolithic ceramics have higher ceramic yield and lower linear shrinkage, but ceramics have functional properties such as high temperature resistance and fracture toughness. needs improvement
The above method will be directly mixed with SiC inorganic ceramic powder to obtain a composite ceramic material, and there will inevitably be interface separation, which will seriously affect the mechanical properties, especially the fracture toughness.

Method used

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  • Molybdenum disilicide/silicon carbide three-dimensional polymer precursor ceramic and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0038] 1. Dissolve 2g of PCS powder in 40mL of xylene, disperse 0.02g of GO powder in 40mL of purified water, and ultrasonically disperse the above two solutions for 30min. Add 0.05mL Castel platinum catalyst to the PCS solution, add 2mL vinyltriethoxysilane and a proper amount of 5wt% dilute hydrochloric acid to the GO dispersion to adjust the pH value of the solution to 1-3.

[0039] 2. Mix the above two solutions into a beaker and place it in a 60°C constant temperature water bath for heating in a water bath, and magnetically stir at a speed of 30 rpm, and keep warm for 30 minutes. After the reaction, the mixture was left to stand for 5 minutes to separate layers, and the upper layer product was taken and subjected to vacuum distillation at 70° C. to obtain PVG solid and ground into powder.

[0040] 3. Take part of the PVG powder and place it in a graphite paper boat and pyrolyze it at 1300°C under the protection of argon atmosphere. The heating rate is 4°C / min, the holding...

Embodiment 2

[0045] 1. Dissolve 2g of PCS powder in 40mL of xylene, disperse 0.02g of GO powder in 40mL of purified water, and ultrasonically disperse the above two solutions for 30min. Add 0.05mL Castel platinum catalyst to the PCS solution, add 2mL vinyltriethoxysilane and a proper amount of 5wt% dilute hydrochloric acid to the GO dispersion to adjust the pH value of the solution to 1-3.

[0046] 2. Mix the above two solutions into a beaker and place it in a 60°C constant temperature water bath for heating in a water bath, and magnetically stir at a speed of 30 rpm, and keep warm for 30 minutes. After the reaction, the mixture was left to stand for 5 minutes to separate layers, and the upper layer product was taken and subjected to vacuum distillation at 70° C. to obtain PVG solid and ground into powder.

[0047] 3. Take part of the PVG powder and place it in a graphite paper boat and pyrolyze it at 1300°C under the protection of argon atmosphere. The heating rate is 4°C / min, the holding...

Embodiment 3

[0052] 1. Dissolve 2g of PCS powder in 40mL of xylene, disperse 0.02g of GO powder in 40mL of purified water, and ultrasonically disperse the above two solutions for 30min. Add 0.05 mL of Custer platinum catalyst to the PCS solution, add 2 mL of vinyltriethoxysilane and an appropriate amount of dilute hydrochloric acid with a concentration of 5 wt % to the GO dispersion to adjust the pH value of the solution to 1-3.

[0053] 2. Mix the above two solutions into a beaker, place in a 60°C constant temperature water bath for heating, and magnetically stir at a speed of 30 rpm, and keep warm for 30 minutes. After the reaction, the mixture was left to stand for 5 minutes to separate layers, and the upper layer product was taken and subjected to vacuum distillation at 70° C. to obtain PVG solid and ground into powder.

[0054] 3. Take part of the PVG powder and place it in a graphite paper boat and pyrolyze it at 1300°C under the protection of argon atmosphere. The heating rate is 4°...

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Abstract

The invention discloses molybdenum disilicide / silicon carbide three-dimensional polymer precursor ceramic and a preparation method thereof, belonging to preparation of ceramic materials. The preparation method comprises the following steps: putting precursor PVG powder into a graphite paper boat and carrying out high-temperature cracking under the protection of an inert atmosphere; mixing MoSi2, cracked SiC(rGO)p ceramic particles and the precursor PVG powder to form a MoSi2 / SiC(rGO)p / PVG mixture, carrying out ball milling and uniform mixing in an alcohol medium, and then drying the MoSi2 / SiC(rGO)p / PVG mixture in an oven; and loading the mixture into a mold for compression molding, conducing demolding to obtain a biscuit, putting the biscuit into an inert atmosphere tube furnace for high-temperature sintering, and conducting cooling along with the furnace to obtain black molybdenum disilicide / silicon carbide three-dimensional polymer precursor ceramic, namely 3D-SiC(rGO, MoSi2x) nanometer composite block ceramic for short, wherein x is the mass fraction of silicon carbide in the whole biscuit. The obtained ceramic is high in heat conductivity and electric conductivity and good in formability and component uniformity; and the preparation method is simple and economical in process.

Description

technical field [0001] The invention relates to the preparation of ceramic materials, in particular to a molybdenum disilicide / silicon carbide three-dimensional polymer precursor ceramic and a preparation method thereof. Background technique [0002] As an advanced ceramic material, silicon carbide (SiC) has excellent mechanical properties, high temperature resistance, thermal shock resistance, chemical stability, corrosion resistance, etc. It also shows good performance under environmental conditions. It is often used to make corrosion-resistant materials, wear-resistant materials, high-temperature-resistant components, high-precision components, etc., in the fields of microelectronic systems, machinery, chemical industry, metallurgy, aerospace, national defense and military industry, etc. All have essential applications. [0003] At present, SiC ceramics can be obtained by normal pressure sintering, hot pressing sintering, reaction sintering and other preparation methods....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/565C04B35/58C04B35/622
CPCC04B35/571C04B35/573C04B35/58092C04B35/622C04B2235/425C04B2235/483C04B2235/6562C04B2235/6567C04B2235/6586C04B2235/96C04B2235/9607C04B2235/9615
Inventor 姚荣迁黄雯燕郑艺浓韩宇宸韩浩哲安子一陈峰
Owner 中科德胜(常州)电子科技有限公司
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