Preparation method of silicon carbide/zirconium carbide composite ceramic

A technology of composite phase ceramics and zirconium carbide, which is applied in the field of preparation of silicon carbide/zirconium carbide composite ceramics, can solve the problems of the mechanical properties and high temperature resistance of the final composite ceramics, and achieve high density ceramics, simple operation, Effects that are easy to engineer

Inactive Publication Date: 2012-06-20
XIAMEN UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a silicon carbide / zirconium carbide composite ceramic for the problems that the introduction of oxygen in the preparation of silicon carbide / zirconium carbide composite ceramics by the existing precursor conversion method leads to the decline of the mechanical properties and high temperature resistance of the final composite ceramics. Preparation method of phase ceramics

Method used

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  • Preparation method of silicon carbide/zirconium carbide composite ceramic
  • Preparation method of silicon carbide/zirconium carbide composite ceramic
  • Preparation method of silicon carbide/zirconium carbide composite ceramic

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Under an inert atmosphere, dissolve zirconocene dichloride with dimethyl sulfoxide, stir, then add liquid hyperbranched polycarbosilane, the mass ratio of zirconocene dichloride and liquid hyperbranched polycarbosilane is 1: 1.

[0025] (2) Under the protection of an inert atmosphere, the mixture obtained in step (1) was distilled off under reduced pressure in vacuum to remove the solvent.

[0026] (3) The mixture obtained in step (2) was cracked at 1400° C. for 120 min under the protection of an inert atmosphere to prepare silicon carbide / zirconium carbide composite ceramics.

[0027] The average molecular formula of the used raw material liquid hyperbranched polycarbosilane is-[SiH 1.26 (CH 3 ) 0.60 (CH 2 CH=CH 2 ) 0.14 CH2 ] n -, as measured by thermogravimetric analysis (TGA), the ceramic yield of liquid hyperbranched polycarbosilane / dichlorozirconocene hybrid precursor at 1400°C is 84.7%, while the raw material liquid hyperbranched polycarbosilane at 140...

Embodiment 2

[0032] (1) Under an inert atmosphere, dissolve zirconocene dichloride with dimethylformamide, stir, then add liquid hyperbranched polycarbosilane, the mass ratio of zirconocene dichloride and liquid hyperbranched polycarbosilane is 1: 2.

[0033] (2) Under the protection of an inert atmosphere, the mixture obtained in step (1) was distilled off under reduced pressure in vacuum to remove the solvent.

[0034] (3) The mixture obtained in step (2) was cracked at 1600° C. for 60 min under the protection of an inert atmosphere to prepare silicon carbide / zirconium carbide composite ceramics.

[0035] The average molecular formula of the used raw material liquid hyperbranched polycarbosilane is-[SiH 1.36 (CH 2 CH 3 ) 0.40 (CH 2 C≡CH) 0.24 CH 2 ] n -, as determined by thermogravimetric analysis (TGA), the ceramic yield of liquid hyperbranched polycarbosilane / dichlorozirconocene hybrid precursor at 1600°C is 76.7%, while the raw material liquid hyperbranched polycarbosilane at ...

Embodiment 3

[0037] (1) Under an inert atmosphere, dissolve zirconocene dichloride with chloroform, stir, then add liquid hyperbranched polycarbosilane, the mass ratio of zirconocene dichloride and liquid hyperbranched polycarbosilane is 1:3.

[0038] (2) Under the protection of an inert atmosphere, the mixture obtained in step (1) was distilled off under reduced pressure in vacuum to remove the solvent.

[0039] (3) The mixture obtained in step (2) was cracked at 1200° C. for 60 minutes under the protection of an inert atmosphere to prepare silicon carbide / zirconium carbide composite ceramics.

[0040] The average molecular formula of the used raw material liquid hyperbranched polycarbosilane is-[SiH(CH 3 )CH 2 ] n -, as determined by thermogravimetric analysis (TGA), the ceramic yield of liquid hyperbranched polycarbosilane / dichlorozirconocene hybrid precursor at 1200°C is 85.2%, while the raw material liquid hyperbranched polycarbosilane at 1200°C The ceramic yield rate is 76.4%, and...

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Abstract

The invention relates to a preparation method of silicon carbide/zirconium carbide composite ceramic, and relates to inorganic nonmetal material composite ceramic. The preparation method comprises the steps of: dissolving bis(cyclopentadienyl) zirconium dichloride with a solvent under the protection of inert atmosphere, and adding liquid hyperbranched polycarbosilane to obtain a mixture A; and distilling the mixture A under reduced pressure under the protection of inert atmosphere to remove the solvent, and carrying out cracking reaction in inert atmosphere to obtain the silicon carbide/zirconium carbide composite ceramic. According to the invention, bis(cyclopentadienyl) zirconium dichloride is used as a zirconium source, and is used for catalyzing the crosslinking reaction of liquid hyperbranched polycarbosilane, so as to increase ceramic yield; zirconium carbide can inhibit the growth of silicon carbide microcrystal grains, and improve high-temperature resistance and oxidation resistance of the composite material; the zirconium content in the composite ceramic can be controlled by controlling the content of bis(cyclopentadienyl) zirconium dichloride in a hybrid precursor; the liquid hyperbranched polycarbosilane/bis(cyclopentadienyl) zirconium dichloride hybrid precursor is free of oxygen, thus the gas escaped in the high-temperature cracking process is reduced; the ceramic has high compactness; and the preparation method is simple to operate, and is easy for engineering.

Description

technical field [0001] The invention relates to an inorganic non-metal material composite ceramic, in particular to a preparation method of a silicon carbide / zirconium carbide composite ceramic. Background technique [0002] Silicon carbide ceramics have the characteristics of wide band gap, high thermal conductivity, high melting point, high electron mobility, high critical breakdown voltage, good chemical stability and low density. It is an ideal material for electronic devices and circuits, and has broad application prospects in many fields such as communications, automobiles, aviation, aerospace and national defense. The precursor conversion method is the main method for preparing silicon carbide ceramics, which was pioneered by Professor Yajima of Tohoku University in Japan in 1975. The common precursor of silicon carbide is polycarbosilane, also known as Yajima polycarbosilane. According to literature reports, silicon carbide ceramics prepared from polycarbosilane pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/56C04B35/565C04B35/622
Inventor 余兆菊杨乐周聪詹俊英涂惠彬廖志楠何国梅夏海平陈立富
Owner XIAMEN UNIV
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