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Ceramic precursor carbon-free polyborosilazane and synthesis method thereof

A technology for polyborosilazane and ceramic precursors, which is applied in the field of ceramic precursor carbon-free polyborosilazane and its synthesis, can solve the problem of high viscosity, no carbon-free polyborosilazane precursor synthesis method, ceramics Unsatisfactory yield and other problems, to achieve the effect of low viscosity, moderate and stable reaction, and good fluidity

Active Publication Date: 2011-06-29
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These are carbopolyborosilazanes, these carbopolyborosilazanes have high viscosity, and the yield of ceramics is not ideal, and the residual carbon atoms in them have a great influence on some special properties of materials, such as dielectric constant, Dielectric loss, etc. will have extremely adverse effects
There is no report on the synthesis method of carbon-free polyborosilazane precursor

Method used

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  • Ceramic precursor carbon-free polyborosilazane and synthesis method thereof
  • Ceramic precursor carbon-free polyborosilazane and synthesis method thereof
  • Ceramic precursor carbon-free polyborosilazane and synthesis method thereof

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Embodiment 1

[0020] (1) 71g borane ammonia complex (H 3 B·NH 3 ) was dissolved in 3000g of diethylene glycol dimethyl ether, and then the solution was heated to 150°C, and the pyrolysis reaction started. Pass the escaped gas through a flask placed in an alcohol bath at 0°C to remove the solvent, cool the remaining gas to -78°C, and collect 53 g of liquid product. The obtained product was further purified by liquid nitrogen to obtain 45 g of relatively pure borazine.

[0021] (2) Add 1000mL pyridine and 100g halosilane H 2 SiCl 2 , the two react to form the by-product H 2 SiCl 2 ·xPy precipitated, passed excess ammonia gas (about 10L) at a flow rate of 100mL / min into the flask, and stopped the reaction after reflux at room temperature for 2h. A large amount of white precipitates were formed in the reaction mixture. After standing for 5 hours, filter under the protection of an inert atmosphere to obtain a pyridine solution of perhydropolysilazane. Distill under reduced pressure (1-3kPa...

Embodiment 2

[0024] (1) borane ammonia complex 71g (H 3 B·NH 3 ) was dissolved in 3500 g of triethylene glycol dimethyl ether, and then the solution was heated to 170°C. The pyrolysis reaction starts. The solvent was removed by passing the evolved gas through the flask placed in an alcohol bath at -10°C. The remaining gas was cooled to -78°C, and 52 g of liquid product was collected. The obtained product was further purified by liquid nitrogen to obtain 49.6 g of relatively pure borazine.

[0025] (2) Add 1500mL pyridine and 130gHSiCl 3 , the two react to form a white complex HSiCl 3 xPy. Pass excess ammonia gas into the flask at a flow rate of 100 mL / min, and stop the reaction after refluxing at 50° C. for 1 h. A large amount of white precipitate formed in the reaction mixture, which was filtered under an inert atmosphere after standing for 5 hours to obtain a pyridine solution of perhydropolysilazane. The solvent pyridine was removed by distillation under reduced pressure (pressu...

Embodiment 3

[0028] The carbon-free polyborosilazane of the present invention contains both Si-N bonds and B-N bonds in its structure, does not contain carbon and other impurity elements except H, and can be cracked to obtain pure silicon nitrogen boron ceramics. Its synthetic method is carried out as follows:

[0029] (1) borane ammonia complex 71g (H 3 B·NH 3 ) was dissolved in 2000 g of tetraethylene glycol dimethyl ether, and then the solution was heated to 200°C. The pyrolysis reaction starts. The solvent was removed by passing the evolved gas through the flask placed in an alcohol bath at -10°C. The remaining gas was cooled to -78°C, and 51.2 g of liquid product was collected. The obtained product was further purified by liquid nitrogen to obtain 50.1 g of relatively pure borazine.

[0030] (2) Add 1000mL pyridine and 80g H 3 SiCl, the two react to form a white complex H 3 SiCl xPy. Pass excess ammonia gas into the flask at a flow rate of 100 mL / min, and stop the reaction aft...

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Abstract

The invention relates to ceramic precursor carbon-free polyborosilazane and a synthesis method thereof. The carbon-free polyborosilazane is a polymer simultaneously containing a Si-N bond and a B-N bond, and pure silicon nitride boron ceramic is obtained after carrying out pyrolysis on the polymer simultaneously containing a Si-N bond and a B-N bond. The carbon-free polyborosilazane obtained by the synthesis method is low in viscosity, good in flowability, and suitable for a precursor dipping-cracking process; and the yield of ceramic is up to 83%, the pyrolysis product is the pure silicon nitride boron ceramic which is suitable for high temperature wave-penetrating materials. The synthesis method of the carbon-free polyborosilazane has the advantages that the operation is simple, the reaction is mitigated and stable, and the controllability is strong.

Description

technical field [0001] The invention relates to a ceramic precursor carbon-free polyborosilazane and a synthesis method thereof. Background technique [0002] 200710035733.9 discloses a preparation method of a polyborosilazane precursor, which includes the following steps: using borohalane, halosilane, and alkylamine compound as starting materials, and the molar ratio of borohalane: halosilane is 1 : 10- 10: 1, the excess proportion of alkylamine is mixed and reacted, and after the reaction is completed, the product is filtered, and the filtrate is low molecular borosilazane, and then the low molecular borosilazane is heated to high molecular weight After cooling, the polyborosilazane precursor can be obtained. Such as 200810031250.6 discloses a kind of preparation method of polyborosilazane precursor. Halosilane, borohalane, and small molecule disilazane are used as starting materials. After mixing according to a certain ratio, the temperature is raised to 150-500°C, and ...

Claims

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Application Information

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IPC IPC(8): C08G77/62C04B35/58
Inventor 李斌张长瑞曹峰王思青李俊生宋阳曦
Owner NAT UNIV OF DEFENSE TECH
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