Method and equipment for preparing precursor body of poly carbon silane ceramics of containing zirconium

A technology of ceramic precursors and polycarbosilane, which is applied in the field of preparation of polycarbosilane ceramic precursors, can solve problems such as single function, complex process equipment, poor ultra-high temperature resistance of SiC ceramics and their fibers, etc., to achieve wide sources, The effect of simple process equipment and easy control of the reaction process

Inactive Publication Date: 2007-10-10
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to overcome the shortcomings of the existing precursor conversion method to prepare SiC ceramics and their fibers with poor ultra-high temperature resistance, single function, and complicated process equipment, etc., to pr

Method used

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  • Method and equipment for preparing precursor body of poly carbon silane ceramics of containing zirconium
  • Method and equipment for preparing precursor body of poly carbon silane ceramics of containing zirconium
  • Method and equipment for preparing precursor body of poly carbon silane ceramics of containing zirconium

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Experimental program
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Effect test

Embodiment 1

[0027] Taking PSCS and zirconium acetylacetonate as raw materials, the mass ratio of the two (the proportions described in the following examples are all mass ratios) is: zirconium acetylacetonate: PSCS=4: 100, 420°C of reaction temperature, and 500°C of cracking temperature , after heat preservation reaction for 6 hours, dissolved in xylene, filtered, and the filtrate was distilled under reduced pressure at 390°C to obtain PZCS with a softening point of 215°C and a zirconium content of 1.31wt%, with a yield of 51.1%. N 2 Heat preservation at 1250°C for 1 hour under atmosphere, and the ceramic yield is 68.3%. Its reaction mechanism is shown in the following formula:

[0028]

[0029] The infrared spectrum, GPC spectrum, and TG spectrum of the PZCS synthesized in this example are shown in Figure 2, Figure 3, and Figure 4, respectively.

Embodiment 2

[0031] Using PCS and tetraethoxy zirconium as raw materials, tetraethoxy zirconium: PCS = 1: 100, the reaction temperature is 450 ° C, the cracking temperature is 450 ° C, and after the reaction time of 1 hour, it is dissolved in xylene and filtered, and the filtrate is at 350 °C for vacuum distillation to obtain PZCS with a softening point of 242 °C and a zirconium content of 0.61 wt%, with a yield of 48.2%. N 2 Heat preservation at 1250°C for 1 hour under atmosphere, and the ceramic yield is 66.5%.

Embodiment 3

[0033] Use PS and zirconium acetylacetonate as raw materials, zirconium acetylacetonate:PS=20:100, reaction temperature 350°C, cracking temperature 550°C, heat preservation reaction time 20h, dissolve in xylene, filter, and distill the filtrate under reduced pressure at 370°C , the softening point is 195 DEG C, the PZCS containing 6.63wt% zirconium is obtained, and the yield is 46.8%. N 2 The temperature was kept at 1250° C. for 1 hour under the atmosphere, and the ceramic yield was 73.5%.

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Abstract

This invention discloses method and apparatus for preparing polycarbosilane ceramic precursor containing Zr. The method comprises: utilizing low molecular weight polymer with S-H bonds (polysilane, polycarbosilane or poly(dimethyl silane)) as the raw material, organic metallic compound containing Zr as the additive, and Ar, N2 or their mixture as the protective atmosphere, and pyrolyzing at high temperatures and normal pressure to obtain Zr-containing SiC ceramic precursor PZCS. The pyrolysis apparatus comprises a three-necked flask in the heater, a pyrolysis column in the electric heating jacket, a condensing tube, a separatory funnel, and a vacuum system seam. The method is simple, and can control the content and properties of Zr in the precursor and the ceramic. The product has such advantages as high purity, high remoldability, and high heat resistance.

Description

technical field [0001] The invention relates to a preparation method and device of a polycarbosilane ceramic precursor containing heterogeneous element zirconium, in particular to a polycarbosilane ceramic precursor containing heterogeneous element zirconium with main chain silicon-containing polymer and zirconium-containing organometallic compound as main raw materials The preparation method and device of the polycarbosilane ceramic precursor. Background technique [0002] With the development of science and technology, national defense, aerospace, energy and other fields have put forward higher and higher requirements for materials such as light weight, high strength, high modulus, high temperature resistance, corrosion resistance, oxidation resistance, and wear resistance. The development of high-performance ceramics and their composite materials to replace traditional high-temperature alloys and refractory metal materials has become the main res...

Claims

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Application Information

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IPC IPC(8): C04B35/571C04B35/622
Inventor 谢征芳曹淑伟王军王浩
Owner NAT UNIV OF DEFENSE TECH
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