Preparation method of polymetal carbosilane precursor

A carbosilane and metal technology, applied in the field of preparation of polymetallic carbosilane precursors, can solve the problems of β-SiC grain growth, large interface stress, high content, etc., and achieve uniform distribution of metal elements and good viscosity stability. The effect of adjustable sex and metal content

Active Publication Date: 2022-03-01
CHANGSHA DAFEI NEW MATERIAL TECH CO LTD
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Problems solved by technology

[0003] Single-phase SiC ceramics have excellent potential for temperature resistance. In theory, pure β-SiC crystals can withstand temperatures up to 2600 °C. The highest temperature resistance of SiC fibers currently prepared is only 1600 °C. The main reason is that the current SiC fibers are not pure. When the temperature rises, the original β-SiC crystallites will get new supplements from the continuous phase and grow rapidly, and the original glassy continuous phase will become an isolation layer for large grains. Large interfacial stress is generated, which reduces the mechanical properties of SiC fibers
At present, the biggest problem that limits the performance improvement of SiC ceramics is: excessive growth of β-SiC grains at

Method used

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  • Preparation method of polymetal carbosilane precursor
  • Preparation method of polymetal carbosilane precursor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Add 20kg of polydimethylsilane to the reactor, and heat up and crack under an inert atmosphere to obtain 18.0kg of liquid polysilocarbosilane, which is called reactant A; 12.0kg of sodium metal and 150kg of xylene are added to another reactor, Raise the temperature to 100°C under a nitrogen atmosphere, stir at high speed for 1 hour to break the metal sodium block into sodium sand, add 6.46kg of dichlorozirconocene, and then slowly add 27.10kg of dichlorodimethylsilyl chloride into the reaction system in the form of dropwise addition , after the dropwise addition, heat up to 135°C, continue to stir for 6 hours until the solution is neutral, cool to room temperature, filter the solution to get the clear liquid, remove xylene, and obtain 24.10kg of reactant B; mix A and B In a reaction kettle with a cracking column and a reflux device, the temperature was raised to 380°C under the protection of nitrogen, kept for 4 hours, and cooled to room temperature to obtain 30.50 kg of...

Embodiment 2

[0044] Add 40kg of polydimethylsilane to the reaction kettle, heat up and crack under an inert atmosphere to obtain 34.8kg of liquid polysilocarbosilane, which is called reactant A; add 11.3kg of metal sodium and 80kg of trimethylbenzene solvent into another reaction kettle , heated up to 100°C under a nitrogen atmosphere, stirred at high speed for 1 hour to break the metal sodium block into sodium sand, added 5.0kg dimethyl zirconocene, and then slowly added 27.10kg dichlorodimethylsilyl chloride in dropwise form The reaction system was heated up to 165°C after the dropwise addition, and continued to stir for 5 hours until the solution was neutral, cooled to room temperature, filtered the solution to obtain the clear liquid, and obtained 20.10kg of reactant B after removing trimethylbenzene; Mix in a reaction kettle with a cracking column and a reflux device, heat up to 410°C under nitrogen protection, keep warm for 5 hours, and cool to room temperature to obtain 36.10kg of cr...

Embodiment 3

[0046] Add 30kg of polydimethylsilane to the reactor, and heat up and crack under an inert atmosphere to obtain 26.8kg of liquid polysilocarbosilane, which is called reactant A; 6.9kg of sodium metal and 60kg of xylene are added to another reactor, Raise the temperature to 100°C under a nitrogen atmosphere, stir at high speed for 1 hour to break the metal sodium block into sodium sand, add 2.5kg of dichlorozirconocene, and then slowly add 17.20kg of dichlorodimethylsilyl chloride into the reaction system in the form of dropwise After the dropwise addition, continue to heat up to 138 ° C, stir for 5 hours until the solution is neutral, cool to room temperature, filter the solution to get the clear liquid, and remove xylene to obtain 12.10 kg of reactant B; mix A and B in In a reaction kettle with a cracking column and a reflux device, heat up to 410°C under the protection of nitrogen, keep it warm for 6 hours, and cool to room temperature to obtain 23.10 kg of crude polyzirconiu...

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Abstract

The invention discloses a preparation method of a polymetal carbosilane precursor, which comprises the following steps: sequentially adding alkali metal and metallocene into an organic solvent in a protective atmosphere, then dropwise adding chlorosilane, carrying out first reaction, solid-liquid separation and solvent removal to obtain a reactant B, and then carrying out second reaction on the reactant B and a reactant A in the protective atmosphere to obtain the polymetal carbosilane precursor. And removing the solvent to obtain polymetal carbosilane, wherein the reactant A is liquid polysilicon carbosilane. According to the preparation method, a large amount of metal is introduced through the reaction of chlorosilane and metallocene, a reactant B which has high reaction activity and contains more Si-Si bonds is obtained at the same time, then the reactant B continues to react with liquid polysilicocarbosilane, and the obtained product has high metal content and good performance stability at the same time. And the distribution of metal elements is uniform, the metal content is adjustable, and the precursor does not contain oxygen.

Description

technical field [0001] The invention relates to a method for preparing a polymetallocarbosilane precursor, and belongs to the technical field of ceramic precursor preparation. Background technique [0002] SiC ceramic fiber is another high-performance fiber after carbon fiber. It has excellent properties such as high strength, high modulus, high temperature resistance, corrosion resistance, oxidation resistance, low density, creep resistance, and good compatibility with ceramic substrates. Due to its excellent high-temperature oxidation resistance, it has become the main reinforcing fiber for the preparation of ultra-high temperature resistant and oxidation-resistant high-performance composite materials. From the perspective of comprehensive performance such as service temperature and oxidation resistance, C f / SiC、SiC f Continuous fiber reinforced ceramic matrix composites represented by / SiC are the preferred materials for ultra-high temperature working parts. At present...

Claims

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Application Information

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IPC IPC(8): C08G77/60C04B35/622C04B35/571
CPCC08G77/60C04B35/571C04B35/62281
Inventor 黄小忠唐云王春齐薛金根段世同龙茜
Owner CHANGSHA DAFEI NEW MATERIAL TECH CO LTD
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