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Method for preparing SiC ceramic precursor for chemical liquid-vapor deposition process

A ceramic precursor and gas phase deposition technology, which is applied in the field of preparing SiC ceramic precursors for chemical liquid vapor deposition process, can solve the problems of high production cost, low deposition efficiency, pollution of environmental equipment, etc., and achieve good fluidity and high deposition efficiency , the effect of low boiling point

Inactive Publication Date: 2012-09-19
UNIV OF SCI & TECH BEIJING +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to develop a SiC ceramic precursor suitable for chemical liquid vapor deposition process and non-corrosive to the environment in view of the problems of long production cycle and high production cost, or low deposition efficiency, pollution of the environment and equipment in the prior art body, and then rapidly prepare C / SiC ceramic matrix composites

Method used

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  • Method for preparing SiC ceramic precursor for chemical liquid-vapor deposition process
  • Method for preparing SiC ceramic precursor for chemical liquid-vapor deposition process

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Effect test

Embodiment 1

[0016] Adopting the present invention to prepare the SiC ceramic precursor for chemical liquid vapor deposition process comprises the following steps:

[0017] 1. Place the polydimethylsilane powder in a three-necked flask equipped with a condenser tube and a receiving device. 2 Heated to 350°C for 4h under protection to obtain liquid carbosilane.

[0018] 2. Filter the liquid carbosilane in (1) to obtain pure carbosilane, and then put it in a normal pressure reactor, under N 2 Heating to 450° C. for 8 hours under protection to obtain a liquid carbosilane precursor crude product.

[0019] 3. After the crude product of the liquid carbosilane precursor is filtered, the filtrate is placed in a normal pressure reactor, and the 2 Heating to 200°C under atmosphere, keeping it warm for 1h, and then performing vacuum distillation under reduced pressure to collect fractions with a boiling point between 100°C and 200°C, with a yield of 45.8%, to obtain a liquid carbosilane precursor. ...

Embodiment 2

[0021] Adopting the present invention to prepare the SiC ceramic precursor for chemical liquid vapor deposition process comprises the following steps:

[0022] 1. Place the polydimethylsilane powder in a three-necked flask equipped with a condenser tube and a receiving device. 2 Heating to 450° C. for 10 h under protection to obtain liquid carbosilane.

[0023] 2. Filter the liquid carbosilane in (1) to obtain pure carbosilane, and then put it in a normal pressure reactor, under N 2 Heating to 500° C. for 20 h under protection to obtain a liquid carbosilane precursor crude product.

[0024] 3. After the crude product of the liquid carbosilane precursor is filtered, the filtrate is placed in a normal pressure reactor, and the 2 atmosphere

[0025] Heating to 200°C under low temperature, keeping it warm for 1h, and then performing vacuum distillation to collect fractions with a boiling point between 100°C and 200°C, with a yield of 38.2%, to obtain a liquid carbosilane precur...

Embodiment 3

[0027] Adopting the present invention to prepare the SiC ceramic precursor for chemical liquid vapor deposition process comprises the following steps:

[0028] 1. Place the polydimethylsilane powder in a three-necked flask equipped with a condenser tube and a receiving device. 2 Heated to 350° C. for 0.5 h under protection to obtain liquid carbosilane.

[0029] 2. Filter the liquid carbosilane in (1) to obtain pure carbosilane, and then put it in a normal pressure reactor, under N 2 Heating to 450° C. for 1 hour under protection to obtain a liquid carbosilane precursor crude product.

[0030] 3. After the crude product of the liquid carbosilane precursor is filtered, the filtrate is placed in a normal pressure reactor, and the 2 Heating to 160°C under the atmosphere, keeping it warm for 3 hours, and then performing vacuum distillation to collect fractions with a boiling point between 100°C and 160°C, with a yield of 52.4%, to obtain a liquid carbosilane precursor.

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Abstract

The invention belongs to the field of inorganic chemistry, and relates to a method for preparing a SiC ceramic precursor for a chemical liquid-vapor deposition process, in particular to a method in which polydimethylsilane is taken as a raw material and which is used for preparing a liquid SiC ceramic precursor for the chemical liquid-vapor deposition process by pyrolysis and distillation processes. The SiC ceramic precursor with the boiling point of 100 to 200 DEG C is obtained by performing pyrolysis and fractionation on the polydimethylsilane at different temperatures. The invention has the advantages that the prepared SiC ceramic precursor for the chemical liquid-vapor deposition process is stable at normal temperature, has low boiling point (below 200 DEG C), is high in flowability and deposition efficiency, and is noncorrosive to the environment, a pyrolysis product is near-stoichiometric beta-SiC, byproducts generated in the deposition and pyrolysis process are noncorrosive andpollution-free to the environment, and the like; and meanwhile, the preparation process is simple, short in preparation period and low in cost.

Description

Technical field: [0001] The invention relates to a method for preparing a SiC ceramic precursor used in a chemical liquid vapor deposition process. In particular, it relates to a method for preparing a liquid SiC ceramic precursor for a chemical liquid vapor deposition process by using polydimethylsilane as a raw material and adopting a pyrolysis and distillation process. Background technique: [0002] C / SiC ceramic matrix composites can be used as high temperature structural materials, thermal protection materials, Brake materials, such as C / SiC throat liners, nozzles and combustion chambers, C / SiC heat exchangers, C / SiC brake discs and brake pads, are used in aerospace, energy, transportation and other fields. [0003] The current methods for preparing C / SiC ceramic matrix composites are mainly precursor impregnation pyrolysis (PIP) and chemical vapor infiltration (CVI). Among them, the precursor impregnation cracking method requires repeated impregnation—more than 10 ti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/622C04B35/565
Inventor 何新波梅敏曲选辉胡海峰张玉娣陈思安李广德张长瑞
Owner UNIV OF SCI & TECH BEIJING