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SiBCN ceramic precursor and synthesis method thereof

A technology of ceramic precursors and synthesis methods, applied in the field of new materials, can solve problems such as by-products that require low temperature conditions, and achieve the effects of high atom utilization, good solubility, and high ceramic yield

Active Publication Date: 2021-06-25
NAT UNIV OF DEFENSE TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The invention provides a SiBCN ceramic precursor and a synthesis method thereof, which are used to overcome the defects in the prior art that the synthesis product is a multi-branched polymer, and the synthesis process requires low temperature conditions and produces a considerable amount of by-products.

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  • SiBCN ceramic precursor and synthesis method thereof
  • SiBCN ceramic precursor and synthesis method thereof
  • SiBCN ceramic precursor and synthesis method thereof

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preparation example Construction

[0023] The present invention proposes a kind of synthetic method of SiBCN ceramic precursor, comprises the following steps:

[0024] S1: Weigh decaborane and organosilicon compound according to the ratio of substances to 1:1;

[0025] S2: dissolving the decaborane in anhydrous tetrahydrofuran to obtain a decaborane solution;

[0026] Dissolving the organosilicon compound in anhydrous tetrahydrofuran to obtain an organosilicon compound solution;

[0027] S3: select a reactor with stirring, replace the air in the reactor with an inert gas, and then add the decaborane solution into the reactor;

[0028] S4: under stirring conditions, add the organosilicon compound solution into the reaction kettle;

[0029] S5: After the feeding is completed, continue to stir at room temperature for 10-20 hours, and then distill under reduced pressure for 10-20 hours under the condition of a constant temperature water bath at 60° C. to remove the solvent to obtain a SiBCN ceramic precursor.

...

Embodiment 1

[0046] The present embodiment provides a kind of synthetic method of SiBCN ceramic precursor, comprises the following steps:

[0047] S1: Weigh 0.1 mol of decaborane and 0.1 mol of 1,3-bis(aminopropyl)tetramethyldisiloxane.

[0048] S2: Dissolving decaborane in anhydrous tetrahydrofuran to obtain a decaborane solution; the concentration of decaborane in the decaborane solution is 0.2 mol / L.

[0049] Dissolve 1,3-bis(aminopropyl)tetramethyldisiloxane in anhydrous tetrahydrofuran to obtain organosilicon compound solution; 1,3-bis(aminopropyl)tetramethyldisiloxane in organosilicon compound solution The molar concentration of ether is 0.2 mol / L.

[0050] S3: Select a reactor with stirring, replace the air in the reactor with nitrogen (introduction speed is 0.5L / min), and then add the decaborane solution to the reactor;

[0051] S4: Under the condition of stirring, add the organosilicon compound solution into the reaction kettle at a rate of 20 mL / min.

[0052] S5: After the add...

Embodiment 2

[0055] The present embodiment provides a kind of synthetic method of SiBCN ceramic precursor, comprises the following steps:

[0056] S1: Weigh 0.1 mol of decaborane and 0.1 mol of [3-(trimethoxysilyl)propyl]ethylenediamine.

[0057] S2: Dissolving decaborane in anhydrous tetrahydrofuran to obtain a decaborane solution; the concentration of decaborane in the decaborane solution is 0.4 mol / L.

[0058] Dissolve [3-(trimethoxysilyl)propyl]ethylenediamine in anhydrous tetrahydrofuran to obtain an organosilicon compound solution; [3-(trimethoxysilyl)propyl]ethylenediamine in the organosilicon compound solution The molar concentration of the amine substance was 0.6 mol / L.

[0059] S3: Select a reactor with stirring, replace the air in the reactor with nitrogen (introduction speed is 1.0L / min), and then add the decaborane solution to the reactor;

[0060] S4: Under the condition of stirring, add the organosilicon compound solution into the reaction kettle at a rate of 10 mL / min.

...

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Abstract

The invention discloses a SiBCN ceramic precursor and a synthesis method thereof.According to the synthesis method of the SiBCN ceramic precursor, decaborane and an organosilicon compound serve as raw materials, the dehydrogenation condensation reaction of the decaborane and the organosilicon compound is utilized, the new SiBCN ceramic precursor is simply and efficiently synthesized, the reaction can be conducted at the room temperature, and the synthesis yield reaches 82 wt% or above. The method has the advantages of no by-product except hydrogen, high atom utilization rate, convenience in large-scale production, good solubility of the synthesized Si-C-N-B multi-element ceramic precursor, high ceramic yield and suitability for various solution processing technologies to prepare ceramic materials with complex shapes.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a SiBCN ceramic precursor and a synthesis method thereof. Background technique [0002] Polyborosilazane is an important precursor for the preparation of multi-component composite ceramic materials. Through different processing and molding methods combined with high-temperature inorganicization, various forms of ceramic materials can be prepared, such as SiBCN ceramic fiber, SiBN ceramic fiber, SiBCN ceramic matrix Composite materials, etc., can also be used to enhance the oxidation resistance of other carbon materials. Researchers at home and abroad have constructed a variety of SiBCN ceramic precursors, some of which are modified by adding boron to the Si-N main chain polymer, and some are directly obtained by the co-ammonolysis polymerization of chlorosilane and chloroborane. Due to the covalent bond formation method of boron, nitrogen, silicon and other elements, these...

Claims

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Application Information

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IPC IPC(8): C08G77/56C08G77/62C08G79/08C04B35/583C04B35/589
CPCC08G77/56C08G77/62C08G79/08C04B35/583C04B35/589
Inventor 邵长伟龙鑫王兵王应德王小宙苟燕子韩成
Owner NAT UNIV OF DEFENSE TECH
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