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Preparation method of poly-zirconium-boron-silazane precursor

A technology of silazane and precursor is applied in the field of preparation of polyzirconium borosilazane precursor, which can solve the problems such as no report on the preparation method of polyzirconium borosilazane precursor, and achieves low price, good processing performance, low cost effect

Inactive Publication Date: 2013-10-02
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, there are no reports on the preparation methods of Si-B-N-C-Zr ceramic precursors or polyzirconium borosilazane precursors

Method used

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  • Preparation method of poly-zirconium-boron-silazane precursor
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  • Preparation method of poly-zirconium-boron-silazane precursor

Examples

Experimental program
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Effect test

Embodiment 1

[0028] This embodiment includes the following steps:

[0029] (1) Weigh 0.15 mol of zirconium tetrachloride, 0.15 mol of boron trichloride, 0.15 mol of trichlorosilane, and 0.9 mol of heptamethyldisilazane;

[0030] (2) Dissolving boron trichloride and trichlorosilane in n-hexane;

[0031] (3) Add the weighed zirconium tetrachloride into a 250ml three-necked flask equipped with a stirrer, a constant pressure funnel, and a distillation device, vacuumize and fill with dry nitrogen for three times, and cool the reactor to minus 15°C;

[0032] (4) Inject the n-hexane solution of boron trichloride and the n-hexane solution of trichlorosilane into a three-necked flask protected by dry nitrogen, then inject heptamethyldisilazane into the constant pressure funnel, and stir while Heptamethyldisilazane was added dropwise in the three-necked flask;

[0033] (5) After the dropwise addition, the reactor was heated to 270°C at a rate of 0.5°C / min, and kept at this temperature for 10 hours...

Embodiment 2

[0040] This embodiment includes the following steps:

[0041] (1) Weigh 1.5 mol of zirconocene dichloride, 0.3 mol of methyl boron dichloride, 0.15 mol of silicon tetrachloride, and 4.5 mol of N-ethylhexamethyldisilazane;

[0042] (2) Dissolving methyl boron dichloride and silicon tetrachloride in cyclopentane;

[0043] (3) Add the weighed zirconocene dichloride into a 500ml three-neck flask equipped with a stirrer, constant pressure funnel, and distillation device, vacuumize and fill with dry nitrogen four times, and cool the reactor to minus 10°C ;

[0044] (4) Inject cyclopentane dissolved in methyl boron dichloride and cyclopentane dissolved in silicon tetrachloride into a three-necked flask protected by dry nitrogen, and then N-ethylhexamethyldisilazane Inject into the constant pressure funnel, and while stirring, add N-ethylhexamethyldisilazane into the three-necked flask in a dropwise manner;

[0045] (5) After the dropwise addition, the reactor was heated to 300°C a...

Embodiment 3

[0049] This embodiment includes the following steps:

[0050] (1) Weigh 0.015 mol of zirconocene dichloride, 0.15 mol of phenyldichloroborane, 0.15 mol of butyltrichlorosilane, and 0.1 mol of N-methylhexaethyldisilazane;

[0051] (2) Dissolving phenyldichloroborane and butyltrichlorosilane in toluene;

[0052] (3) Add the weighed zirconocene dichloride into a 250ml three-neck flask equipped with a stirrer, constant pressure funnel, and distillation device, vacuumize and fill with dry nitrogen four times, and cool the reactor to minus 10°C ;

[0053] (4) Inject the toluene dissolved in phenyldichloroborane and the toluene dissolved in butyltrichlorosilane into a three-necked flask protected by dry nitrogen, and then pour the obtained N-methylhexaethyldisilazane Inject it into a constant pressure funnel, and while stirring, add N-methylhexaethyldisilazane into the three-necked flask in a dropwise manner;

[0054] (5) After the dropwise addition, the reactor was heated to 320°...

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Abstract

A preparation method of a poly-zirconium-boron-silazane precursor comprises the following steps: 1, weighing an organic zirconium compound, boron haloalkane, halogenosilane and micromolecular disilazane at the molar ratio of 1:(0.1-10):(0.1-10):(3-30); 2, respectively dissolving the boron haloalkane and the halogenosilane in organic solvents; 3, adding the organic zirconium compound to a reaction vessel, vacuumizing, filling dry nitrogen gas and precooling the reaction vessel; 4, adding the organic solvent of the boron haloalkane adn the organic solvent of the halogenosilane to the reaction vessel, and dripping the micromolecular disilazane in the reaction vessel; 5, after the dripping is finished, heating the reaction vessel to 150-500 DEG C, and preserving heat for 2-30 hours; 6, cooling the reaction vessel to 120-350 DEG C, distilling under reduced pressure and cooling to the room temperature. The poly-zirconium-boron-silazane precursor prepared according to the method is especially suitable for preparing ultra-high temperature ceramic materials.

Description

technical field [0001] The invention relates to a preparation method of a polyzirconium borosilazane precursor, in particular to a preparation method of a multi-element ceramic precursor containing Si, B, N, C, Zr and other elements. Background technique [0002] Multi-component ceramics containing Si, B, N, C, Zr and other elements have excellent high temperature strength, high modulus, excellent high temperature oxidation resistance and high temperature creep resistance. Therefore, Si-B-N-C-Zr system ceramics are used in aviation, Aerospace, weapons, ships and other fields that require high strength, high modulus, high temperature resistance, oxidation resistance, thermal shock resistance, high temperature creep resistance materials have important application prospects. [0003] Ultra-High-Temperature Ceramics (UHTC) ( Adv. Mater. Process , 2010, 168(6):26-28), generally refers to ceramic materials that can be used at temperatures above 1800 °C for a long time, and can ad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/62C04B35/58
Inventor 邵长伟王浩王军谢征芳宋永才苟燕子
Owner NAT UNIV OF DEFENSE TECH
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