A liquid curable boron-containing polycarbosilane and its preparation method
A technology of polycarbosilane and polysilicon carbosilane is applied in the field of liquid curable boron-containing polycarbosilane and its preparation, which can solve the problems of uneven distribution of boron elements, complicated preparation processes, etc. High temperature resistance, the effect of avoiding phase separation of ceramic products
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[0023] An aspect of the embodiments of the present invention provides a method for preparing a liquid curable boron-containing polycarbosilane, comprising:
[0024] In a closed reaction vessel, the polysilicon carbosilane and the boron-containing monomer are subjected to a first reaction to generate a liquid boron-containing polycarbosilane, wherein the polysilicon carbosilane is a low molecular weight obtained by pyrolysis of polydimethylsilane at high temperature. The product is liquid at room temperature and has a molecular weight of less than 1000 g / mol;
[0025] The second reaction is carried out in a uniformly mixed reaction system comprising the liquid boron-containing polycarbosilane, the C=C bond-containing organosilicon compound and the catalyst to obtain a liquid curable boron-containing polycarbosilane.
[0026] In some embodiments, the liquid boron-containing polycarbosilane is formed by the reaction of polysilicon carbosilane and a boron-containing monomer in a clo...
Embodiment 1
[0048] Polydimethylsilane is pyrolyzed at high temperature to obtain polysilicon carbosilane, which has a molecular weight of 500 g / mol and is liquid at room temperature. Add 300g of liquid polysilicon carbosilane and 6g of carborane into the closed device, replace the kettle with high-purity nitrogen three times, and seal the device; then, turn on the heating, raise the temperature to 320°C at a certain heating rate, and stop after 2 hours of reaction. When it is lowered to room temperature, take out the reactant liquid boron-containing polycarbosilane LPBCS01;
[0049] Mix 100 g of the above LPBCS01 and 80 g of tetramethyltetravinylcyclotetrasilazane, add 0.001 g of chloroplatinic acid, stir evenly at 80°C and react for 1 min to obtain a liquid curable boron nitrogen-containing polycarbosilane LSiBCN.
[0050] The boron-nitrogen-containing polycarbosilane gel SiBCN is obtained by curing the above LSiBCN at 200-300° C. for 1-3 hours in a nitrogen atmosphere.
[0051] figure...
Embodiment 2
[0054] Mix 100 g of LPBCS01 and 75 g of tetramethyltetravinylcyclotetrasiloxane in the above Example 1, add 0.002 g of chloroplatinic acid, stir evenly at 60 ° C for 10 min, and obtain a liquid curable boron-oxygen-containing polycarbosilane LSiBCO .
[0055] The above-mentioned LSiBCO is cured under nitrogen atmosphere at 200-300° C. for 1-3 hours to obtain boron-oxygen-containing polycarbosilane gel SiBCO.
[0056] The viscosity of LSiBCO was determined to be 38 mPa·S by viscometer, and the ceramic yield of SiBCO gel under nitrogen atmosphere at 1000° C. was 75% by thermogravimetric analysis.
[0057] The LSiBO precursor is suitable as a precursor of boron-oxygen-containing SiC ceramics.
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Abstract
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