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Si/C/Zr ceramic precursor and preparation method thereof

A technology of ceramic precursors and monomers, applied in the field of ceramic materials, can solve problems such as lack of processability, and achieve the effects of high synthesis yield and product purity, small curing heat release, and simple and easy synthesis process.

Inactive Publication Date: 2014-05-07
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Xiamen University will Cp 2 ZrCl 2 Reaction with allyl hydrogen polycarbosilane to prepare Si / C / Zr ceramic precursor, this precursor can obtain higher ceramic yield, but the precursor is solid and insoluble in organic solvents, and does not have processability

Method used

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  • Si/C/Zr ceramic precursor and preparation method thereof
  • Si/C/Zr ceramic precursor and preparation method thereof
  • Si/C/Zr ceramic precursor and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0040] 500ml dry three-neck bottle, equipped with N 2 Import piston, condensation tube, nitrogen outlet piston, constant pressure dropping funnel and electromagnetic force stirring, vacuumize, and replace the air in the system with nitrogen gas, and bake with alcohol lamp to remove adsorbed water. Add 4.0g of magnesium chips into the reaction flask, add 50ml of tetrahydrofuran into the reaction flask with a syringe; add 100ml of tetrahydrofuran, 1.0g (0.013mol) of allyl chloride, 10.6g (0.06mol) of methanol into the constant pressure dropping funnel Chlorosilane, 17.5g (0.06mol) zirconocene dichloride to form a mixed solution. At 60°C, slowly add the mixed solution dropwise into the mixed system of magnesium chips and tetrahydrofuran under stirring, and continue stirring for 10 h after the dropwise addition is completed. Add 1.25 g of granular lithium aluminum hydride and stir at room temperature for 5-20 hours.

[0041] Add 100ml of petroleum ether, 350ml of deionized water...

Embodiment 2

[0048] 500ml dry three-neck bottle, equipped with N 2 Import piston, condensation tube, nitrogen outlet piston, constant pressure dropping funnel and electromagnetic force stirring, vacuumize, and replace the air in the system with nitrogen gas, and bake with alcohol lamp to remove adsorbed water. Add 4.0g of magnesium chips to the reaction flask, add 50ml of tetrahydrofuran to the reaction flask with a syringe; add 100ml of tetrahydrofuran, 1.0g (0.013mol) of allyl chloride, 15.8g (0.09mol) of methanol to the constant pressure dropping funnel Chlorosilane, 8.8g (0.03mol) zirconocene dichloride and 2.2g (0.013mol) chloromethylmethyldichlorosilane form a mixed solution. At 60°C, slowly add the mixed solution dropwise into the mixed system of magnesium chips and tetrahydrofuran under stirring, and continue stirring for 10 h after the dropwise addition is completed. Add 1.9 g of granular lithium aluminum hydride and stir at room temperature for 5-20 hours.

[0049] Add 100ml of...

Embodiment 3

[0055] 500ml dry three-neck bottle, equipped with N 2 Import piston, condensation tube, nitrogen outlet piston, constant pressure dropping funnel and electromagnetic force stirring, vacuumize, and replace the air in the system with nitrogen gas, and bake with alcohol lamp to remove adsorbed water. Add 4.0g of magnesium chips to the reaction bottle, add 50ml of tetrahydrofuran to the reaction bottle with a syringe; add 100ml of tetrahydrofuran, 2.0g (0.026mol) of allyl chloride, 21.1g (0.12mol) of methanol to the constant pressure dropping funnel Chlorosilane, 8.8g (0.03mol) zirconocene dichloride and 4.3g (0.026mol) chloromethylmethyldichlorosilane form a mixed solution. At 60°C, slowly add the mixed solution dropwise into the mixed system of magnesium chips and tetrahydrofuran under stirring, and continue stirring for 10 h after the dropwise addition is completed. Add 2.5 g of granular lithium aluminum hydride and stir at room temperature for 5-20 hours.

[0056] Add 100ml ...

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Abstract

The invention relates to a Si / C / Zr ceramic precursor and a preparation method thereof, and belongs to the technical field of a ceramic material. The Si / C / Zr ceramic precursor is prepared by adopting a Grignard coupling reaction method; Si and Zr elements can be simultaneously introduced to a main polymer chain at an atomic level so as to obtain a silicon-zirconium integrated polymer; a synthetic technology is simple and practicable; and the synthetic yield and the purity of the product are relatively high. A reaction raw material, namely polycarbosilane used in the preparation method contains Si-H bonds and C is equivalent to C bonds, has good thermosetting property and is small in curing heat release, low in curing weight loss and good in manufacturability; the polycarbosilane self is cross-linked and cured at a certain temperature; and the ceramic yield is high and can reach 60-70%. The Si / C / Zr ceramic precursor can be applied to a superhigh temperature ceramic matrix composite steeping matrix, can also be used for preparation of high performance materials such as Si / C / Zr ceramic coatings and fibers and has wide application.

Description

technical field [0001] The invention relates to a Si / C / Zr ceramic precursor and a preparation method thereof, belonging to the technical field of ceramic materials. Background technique [0002] SiC ceramics have excellent properties such as high strength, high modulus, high temperature resistance, corrosion resistance, oxidation resistance, and low density. Wide range of uses. At present, SiC ceramics are mainly prepared by precursor conversion method. The precursor conversion method is a method and process in which an organic polymer is used as a precursor, and after being molded by using its soluble and fusible characteristics, it is subjected to high-temperature thermal decomposition treatment to transform it from an organic material into an inorganic ceramic material. Such organic polymers are called organic precursors or ceramic precursors. [0003] With the development of science and technology, higher requirements are put forward for the performance of SiC ceramic...

Claims

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Application Information

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IPC IPC(8): C08G77/60C07F17/00C04B35/56C04B35/565C04B35/622
Inventor 胡继东陶孟李军平冯志海
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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