Liquid curable boron-containing polycarbosilane and preparation method thereof

The 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 process, etc. Simple process and the effect of increasing compactness

Active Publication Date: 2020-01-17
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned method for preparing boron-containing polycarbosilane fibers also has problems such as uneven distribution of boron elements or complicated preparation processes.

Method used

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  • Liquid curable boron-containing polycarbosilane and preparation method thereof
  • Liquid curable boron-containing polycarbosilane and preparation method thereof
  • Liquid curable boron-containing polycarbosilane and preparation method thereof

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[0023] A method for preparing a liquid curable boron-containing polycarbosilane provided by an aspect of the embodiments of the present invention includes:

[0024] In an airtight reaction vessel, polysilocarbosilane and boron-containing monomers are subjected to the first reaction to generate liquid boron-containing polycarbosilane, wherein the polysilocarbosilane is a low-molecular-weight polydimethylsilane cracked at high temperature The product is liquid at room temperature and has a molecular weight of less than 1000g / mol;

[0025] The uniformly mixed reaction system comprising liquid boron-containing polycarbosilane, organosilicon compound containing C=C bond and catalyst is subjected to the second reaction to obtain liquid curable boron-containing polycarbosilane.

[0026] In some embodiments, the liquid boron-containing polycarbosilane is formed by reacting polysilocarbosilane and boron-containing monomers in a closed system, and is in a liquid state at room temperature,...

Embodiment 1

[0048] Polydimethylsilane is cracked at high temperature to obtain polysilocarbosilane, which has a molecular weight of 500 g / mol and is liquid at room temperature. Add 300g of liquid polysilocarbosilane and 6g of carborane into the closed device, replace the kettle with high-purity nitrogen three times, and then seal the device; then, start the temperature rise, and raise the temperature to 320°C at a certain heating rate, and stop the reaction after 2 hours. 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 and react at 80°C for 1 min to obtain liquid curable boron-nitrogen-containing polycarbosilane LSiBCN.

[0050] The above-mentioned LSiBCN is cured at 200-300° C. for 1-3 hours under a nitrogen atmosphere to obtain boron-nitrogen-containing polycarbosilane gel SiBCN.

[00...

Embodiment 2

[0054] Take 100g of LPBCS01 and 75g of tetramethyltetravinylcyclotetrasiloxane in the above example 1 and mix them, add 0.002g of chloroplatinic acid, stir evenly and react at 60°C for 10min to obtain a liquid curable boron-oxygen-containing polycarbosilane LSiBCO .

[0055] The above-mentioned LSiBCO is cured at 200-300° C. for 1-3 hours under a nitrogen atmosphere to obtain boron-oxygen-containing polycarbosilane gel SiBCO.

[0056] The viscosity of LSiBCO measured by a viscometer is 38mPa·S, and the ceramic yield of SiBCO gel is 75% at 1000°C under a nitrogen atmosphere by thermogravimetric analysis.

[0057] The LSiBO precursor is suitable as a precursor of boron-oxygen-containing SiC ceramics.

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Abstract

The invention discloses liquid curable boron-containing polycarbosilane and a preparation method thereof. The preparation method comprises the following steps: in a closed reaction container, subjecting polycarbosilane and a boron-containing monomer to a first reaction to generate liquid boron-containing polycarbosilane, wherein the polycarbosilane is a low-molecular-weight product obtained afterhigh-temperature cracking of polydimethylsilane, is in a liquid state at room temperature, and has a molecular weight of less than 1000 g / mol; and carrying out a second reaction on a uniformly-mixed reaction system containing the liquid boron-containing polycarbosilane, an organosilicon compound containing a C=C bond and a catalyst to obtain the liquid curable boron-containing polycarbosilane. Theliquid curable boron-containing polycarbosilane precursor disclosed by the invention is in a liquid state at room temperature, is simple in preparation process and long in storage time, can be thermocured, and is applicable to the fields of preparation of silicon carbide ceramic-based composite materials, high-temperature-resistant coatings, adhesives and the like through a precursor infiltrationand pyrolysis (PIP) method; and due to the existence of boron, the temperature resistance of a final product is improved.

Description

technical field [0001] The invention belongs to the technical field of ceramic precursor preparation, and in particular relates to a liquid curable boron-containing polycarbosilane and a preparation method thereof. Background technique [0002] Polymer-derived ceramics (Polymer Derived Ceramics, PDCs) are organic polymers prepared by chemical synthesis that can be converted into ceramic materials by pyrolysis, converted into thermosetting polymers by cross-linking and curing, and then obtained by high-temperature cracking to ceramics. One of the hot research materials in the world. Compared with the traditional ceramic preparation process, PDCs have the advantages of designing the precursor structure, good manufacturability and processability, and lower preparation temperature. Silicon carbide (SiC) ceramics have excellent properties such as high temperature resistance, oxidation resistance, high thermal conductivity, and corrosion resistance, and have important application...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60C04B35/571C04B35/58C04B35/622C09D183/16C09J183/16
CPCC08G77/60C04B35/571C04B35/58C04B35/622C09D183/16C09J183/16
Inventor 莫高明宋育杰陈海俊何流黄庆黄政仁
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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