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Organometallic polymer composite ceramic precursor and preparation method and application thereof

A multiphase ceramic and organometallic technology, which is applied in the field of organometallic polymer multiphase ceramic precursors and their preparation, can solve the problems of difficult and impossible to achieve effective infiltration, doping and bonding of ZrC ceramics, and achieve good resistance. high temperature effect

Active Publication Date: 2016-06-15
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the above methods can successfully prepare ZrC ceramics, it is difficult to combine with the preparation process of fiber-reinforced ceramic matrix composites, and it is impossible to truly realize the effective infiltration and doping of ZrC ceramics in the matrix of ceramic matrix composites.

Method used

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  • Organometallic polymer composite ceramic precursor and preparation method and application thereof
  • Organometallic polymer composite ceramic precursor and preparation method and application thereof
  • Organometallic polymer composite ceramic precursor and preparation method and application thereof

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preparation example Construction

[0041] Another aspect of the present invention also provides a kind of preparation method of above-mentioned precursor, comprises the following steps:

[0042] A4 monomers and B-type monomers undergo copolymerization reactions to prepare precursors;

[0043] The A4 monomer is zirconium tetraallylamide, titanium tetraallylamide or hafnium tetraallylamide; the type B monomer is polycarbosilane or polymethylsilane.

[0044]The organometallic polymer ceramic precursor of the present invention is prepared by copolymerizing organometallic zirconium A4 monomers containing double bonds and type B monomers. The A4 monomer here can be various types of organometallic zirconium monomers containing double bonds. Type B monomers can be various types of boron-containing monomers. The precursor can be prepared by reacting the two according to conventional copolymerization reaction conditions.

[0045] Preferably, the A4 monomer and the B-type monomer are mixed in a molar ratio of 4:1-16 fo...

Embodiment 1

[0068] Under nitrogen protection, add 1.1g of tetraallylamino zirconium (A4 monomer) and 50ml of toluene to the three-necked flask, and keep the temperature at -20°C; Body and PMS mass ratio is 1:6), reacted for 48 hours, the solution became viscous; add 100ml of n-hexane, precipitate and filter, dry at 80°C, remove solvent, and obtain Zr-Si-C-N organometallic polymer composite ceramic precursor Yellow block. Yield 72%.

[0069] The resulting ceramic precursor polymer is soluble in DMF, NMP and DMSO. The structure of the precursor was characterized and tested by IR and TGA. In the IR spectrum, 1257cm-1 represents Si–CH 3 The vibration absorption peak of 1120cm -1 Represents the shock absorption peak of N–C (see figure 1 ). The vibrational peaks shown in the figure can prove that the structure of the precursor polymer is consistent with the molecular design. The TGA test result shows that this precursor polymer is in argon atmosphere, and the ceramic production rate of 14...

Embodiment 2

[0072] The difference from Example 1 is that the raw material A4 monomer is hafnium tetraallylamide, and the molar ratio to B monomer is 3:4, and the rest is the same as in Example 1. The obtained product is a light yellow block with a yield of 68%.

[0073] The resulting ceramic precursor polymer is soluble in DMF, NMP and DMSO. Put the Hf-Si-C-N ceramic precursor polymer in an inert atmosphere, crack it at a high temperature of 1400°C for 2 hours, and obtain Hf-Si-C-N ceramics with a yield of 62%. The ultra-high temperature resistant component HfC in the prepared ceramics The / SiC content reached 78%; no obvious weight loss was seen after 2 hours of treatment at 2000 °C.

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Abstract

The invention provides an organometallic polymer composite ceramic precursor and a preparation method and application thereof.The organometallic polymer composite ceramic precursor can be used to prepare Zr-Si-C-N ceramics, the yield of the ceramics is 40-60%, no evident weight loss is discovered when the ceramics are processed at 2000 DEG C for 2 hours, and the ceramics are good in high temperature resistance.The ceramics are promising in application prospect in fields such as aviation and supersonic aircrafts.

Description

technical field [0001] The invention relates to the technical field of ultra-high temperature resistant ceramics, in particular to an organometallic polymer composite ceramic precursor and its preparation method and application. Background technique [0002] With the rapid development of high-tech fields such as aerospace, higher and higher requirements are placed on material performance. For example, modern aircraft must be able to adapt to extreme environments such as supersonic long-duration flight, atmospheric re-entry, and transatmospheric flight, especially key parts or components such as aircraft nose cones, wing leading edges, and engine hot ends. Not only must they withstand temperatures above 2000 °C (Even as high as 3000°C) ultra-high temperature, but also have air oxidation resistance, erosion resistance, thermal shock resistance, etc. Among them, the ultra-high temperature resistance and ultra-high temperature oxidation resistance of the material are the key. I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60C04B35/58
CPCC04B35/58C04B35/622C04B2235/483C08G77/60
Inventor 王军陈树刚王浩简科邵长伟王小宙
Owner NAT UNIV OF DEFENSE TECH
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