A kind of zr-c-si polymer ceramic precursor and its preparation method and application

A ceramic precursor, zr-c-si technology, which is applied in the field of Zr-C-Si polymer ceramic precursor and its preparation and application, can solve the problems of harsh conditions, complicated preparation process and high reaction temperature, and achieve good resistance. High temperature performance, broad application prospects, and the effect of simple synthesis process

Active Publication Date: 2011-12-07
NAT UNIV OF DEFENSE TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation process of the ceramics prepared by the above three precursor methods is complicated, the reaction temperature is high, the conditions are harsh, and the energy consumption is high. Poor, can not reach the high temperature above 2000 degrees required by ultra-high temperature resistant ceramics
There is no report on the preparation method and application of Zr-C-Si polymer ceramic precursor

Method used

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  • A kind of zr-c-si polymer ceramic precursor and its preparation method and application
  • A kind of zr-c-si polymer ceramic precursor and its preparation method and application
  • A kind of zr-c-si polymer ceramic precursor and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Under nitrogen protection, add 0.55 g (0.002 mol) divinylzirconocene (A 2 monomer), 1.1g PCS (ie A 2 The mass ratio of monomer and PCS is 1:2 and 10 ml of toluene, the temperature is kept at 60-90 ° C, reacted for 48 hours under electromagnetic stirring, and the solution becomes viscous; add 90 ml of n-pentane, precipitate, filter, and put in a vacuum oven for 80 ℃ drying, to obtain Zr-C-Si ceramic precursor polymer (see figure 1 ). Yield 96%.

[0024] The obtained Zr-C-Si ceramic precursor polymer is soluble in DMF, NMP, DMAc and DMSO. In the IR spectrum, 2953 cm -1 and 2898 cm -1 are the carbon-hydrogen vibration absorption peaks on the methyl group and methylene group on the precursor polymer; 2099 cm -1 It is the characteristic absorption peak of the silicon-hydrogen bond on the main chain of the precursor polymer; 1650 cm -1 It is the characteristic absorption peak of carbon-carbon double bond; 1389 cm -1 and 1253 cm -1 It is the characteristic absorpt...

Embodiment 2

[0027] and The difference of embodiment 1 is only that raw material A 2 The mass ratio of monomer and PCS is 1:8. Under nitrogen protection, add 0.55 g (0.002 mol) divinylzirconocene (A 2 monomer), 4.4g PCS (ie A 2 The mass ratio of monomer and PCS is 1:8 and 18 ml of toluene, the temperature is kept at 70-80 ° C, reacted under electromagnetic stirring for 40 hours, the solution becomes viscous; add 180 ml of n-pentane, precipitate, filter, and put in a vacuum oven for 80 ℃ drying, the obtained Zr-C-Si ceramic precursor polymer is orange polymer powder. Yield 95%.

[0028] The obtained Zr-B-C ceramic precursor polymer is soluble in DMF, NMP, DMAc and DMSO. The Zr-C-Si ceramic precursor polymer is placed in nitrogen, cracked at a high temperature, the cracking temperature is controlled at 1700°C, and the cracking time is 1.5 hours to obtain Zr-C-Si ceramics. The ceramic yield is 54%. The ZrC / SiC content of the ultra-high temperature resistant component in the prepared Z...

Embodiment 3

[0030] The only difference with Example 1 is that raw material A 2 The monomer is changed from divinyl zirconocene to dipropenyl zirconocene, and the remainder is the same as in Example 1. Under the protection of nitrogen, add 0.606 g of dipropenylzirconocene (A 2 monomer), 0.606g PCS (ie A 2The mass ratio of monomer and PCS is 1:1 and 10 ml of toluene, the temperature is kept at 70-90 ° C, reacted for 45 hours under electromagnetic stirring, the solution becomes viscous; add 100 ml of n-pentane, precipitate, filter, and put in a vacuum oven for 80 ℃ drying, the obtained Zr-C-Si ceramic precursor polymer is orange-red polymer powder. Yield 92%. The obtained Zr-C-Si ceramic precursor polymer is soluble in DMF, NMP, DMAc and DMSO. The Zr-C-Si ceramic precursor polymer is placed in nitrogen, cracked at a high temperature, the cracking temperature is controlled at 1300° C., and the cracking time is 2 hours to obtain Zr-C-Si ceramics. The ceramic yield is 45%. The ZrC / SiC con...

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Abstract

The invention discloses a Zr-C-Si polymer ceramic precursor and a preparation method and application thereof. The Zr-C-Si polymer ceramic precursor is prepared by performing graft copolymerization on a double-bond organic metal zirconium monomer and polycarbosilane (PCS). The Zr-C-Si polymer ceramic precursor is used for preparing Zr-C-Si ceramic, the yield of ceramic is up to 50-65 percent, the content of ZrC and the content of SiC in a prepared ceramic material are higher than 70 percent by weight, and high high-temperature resistance is achieved. The Zr-C-Si polymer ceramic precursor can meet the requirement on temperature over 2,000 DEG C which is needed by ultrahigh-temperature ceramic, and has wide application prospect in the fields of aero-space, supersonic aircrafts, reentrant aircrafts and the like, a simple synthesis process and low energy consumption.

Description

technical field [0001] The invention relates to a Zr-C-Si polymer ceramic precursor and its preparation method and application. Background technique [0002] Precursor conversion method is the most ideal method for preparing ultra-high temperature resistant ceramic matrix composites. There have been many reports on the preparation methods of existing ceramic precursors, such as CN200810031049.8 discloses a preparation method of SiC ceramic precursors containing niobium, which includes (1) a low molecular weight polymer equivalent to the main chain containing silicon The niobium metal chloride or organic compound of 0.5wt%-20wt% by weight is placed in a three-necked flask, and the low molecular weight polymer containing silicon in the main chain is placed in this three-necked flask to cover the niobium metal chloride or organic compound; (2) in Ar or N 2 Under protection, according to the heating rate of 0.1-5°C / min, the temperature of the material in the three-necked flask...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60C04B35/515
Inventor 王浩陈兴波王军高波王应德薛金根谢征芳简科
Owner NAT UNIV OF DEFENSE TECH
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