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SiC-ZrC-ZrB2 nano complex phase ceramic modified C/C composite material and preparation method thereof

A technology of multiphase ceramics and composite materials, which is applied in the field of C/C composite materials, can solve the problems of difficult uniform distribution of ceramic particles, reduce the high temperature performance of C/C composite materials, etc., achieve good physical and chemical compatibility, improve Mechanical properties, the effect of enhancing self-healing antioxidant capacity

Inactive Publication Date: 2014-12-24
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are two problems in the specific implementation process: (1) It is difficult to achieve a uniform distribution of ceramic particles in the matrix carbon and carbon fiber bundles, thus limiting the synergistic oxidation resistance between various ceramic components to a large extent. (Paul P. P., Schwab S.T. Obtaining carbon materials and their oxidation resistance through metal-organic modification of pitch. Charcoal, 1996, 34 (1): 89-95); (2) The addition of anti-oxidation ceramic particles is usually At the expense of reducing the high temperature performance of C / C composites

Method used

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  • SiC-ZrC-ZrB2 nano complex phase ceramic modified C/C composite material and preparation method thereof
  • SiC-ZrC-ZrB2 nano complex phase ceramic modified C/C composite material and preparation method thereof

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preparation example Construction

[0041] The preparation steps of the ZrC precursor are as follows: vacuumize the reactor to 0.06-0.08MPa, feed argon to normal pressure, then add toluene, zirconium salt and absolute ethanol to the reactor in sequence, and stir evenly. Wherein: the molar ratio of zirconium salt: toluene: absolute ethanol is 1: (3~5): (4~10); then feed ammonia gas under the condition of -10~10°C, and the flow rate of feeding ammonia gas is 40~60ml / min, react for 2~6h, and filter to obtain a toluene solution of zirconium alkoxide.

[0042] The reactor is evacuated to 0.06~0.08MPa, argon is introduced to normal pressure, and then the toluene solution of zirconium alkoxide, β-diketone and phenol are sequentially added to the reactor, and stirred evenly, wherein: β-diketone: phenol: The molar ratio of zirconium salt is (1~4):(2~4):1; then the reaction system is heated to 120~300°C at a heating rate of 2~4°C / min, kept for 1~10h, and depressurized Distill and cool to room temperature to obtai...

Embodiment 1

[0044] A SiC-ZrC-ZrB 2 A nanocomposite ceramic modified C / C composite material and a preparation method thereof. The concrete steps of described preparation method are:

[0045] Step 1. Pretreatment of carbon fiber preform

[0046] The carbon fiber preform was washed with acetone for 30-60 minutes, and dried at 70-100°C for 1-2 hours to obtain a pretreated carbon fiber preform.

[0047] Step 2, preparation of borosilicate zirconium doped pitch

[0048] Dissolve the asphalt in toluene first, let it stand at room temperature for 1~2h, separate the solid and liquid, and distill the solution after the solid-liquid separation at 110~150°C to obtain the asphalt toluene soluble component.

[0049] Mix 1-2wt% organic boron, 5-6wt% organic silicon, 10-12wt% ZrC precursor and 80-84wt% asphalt toluene soluble components to obtain the mixture. Add a solvent to the mixture, the mass ratio of the mixture to the solvent is 1:(1~2), stir magnetically for 0.5~1h, and the mixture is obt...

Embodiment 2

[0064] A SiC-ZrC-ZrB 2 A nanocomposite ceramic modified C / C composite material and a preparation method thereof. The concrete steps of described preparation method are:

[0065] Step 1 is the same as Step 1 in Embodiment 1.

[0066] Step 2, preparation of borosilicate zirconium doped pitch

[0067] Dissolve the asphalt in toluene first, let it stand at room temperature for 1~2h, separate the solid and liquid, and distill the solution after the solid-liquid separation at 110~150°C to obtain the asphalt toluene soluble component.

[0068] Mix 2-3wt% organoboron, 6-7wt% organosilicon, 12-14wt% ZrC precursor and 76-80wt% asphalt toluene soluble components to obtain the mixture. Add a solvent to the mixture, the mass ratio of the mixture to the solvent is 1:(1~2), stir magnetically for 0.5~1h, and the mixture is obtained. Then the mixed solution is transferred to the reaction kettle, and an inert gas is introduced, and the reaction kettle is heated to 300~350°C at a heating...

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Abstract

The invention relates to a SiC-ZrC-ZrB2 nano complex phase ceramic modified C / C composite material and a preparation method thereof. A technical scheme adopted by the invention is that the preparation method of the SiC-ZrC-ZrB2 nano complex phase ceramic modified C / C composite material comprises the following steps: mixing 1-5wt% of organic boron, 5-10wt% of organic silicon, 10-20wt% of a ZrC precusor and 65-84wt% of an asphalt methylbenzene soluble component, adding a solvent to dissolve the mixture, reacting the obtained solution for 1-4 hours at 300-450 DEG C to obtain boron-silicon-zirconium-doped asphalt; dipping a carbon fiber prefabricated body with the boron-silicon-zirconium-doped asphalt, and then carrying out pyrolysis treatment to obtain a SiC-ZrC-ZrB2 nano complex phase ceramic modified C / C perform body; and repeatedly dipping and carrying out pyrolysis treatment on the SiC-ZrC-ZrB2 nano complex phase ceramic modified C / C perform body until the density is 1.9-2.5g / cm<3> to obtain the SiC-ZrC-ZrB2 nano complex phase ceramic modified C / C composite material. The composite material prepared by the preparation method has good mechanical performance, self-healing antioxidant ability and superhigh temperature ablation resistance within a wider temperature range.

Description

technical field [0001] The invention belongs to the technical field of C / C composite materials. involving a SiC-ZrC-ZrB 2 A nanocomposite ceramic modified C / C composite material and a preparation method thereof. Background technique [0002] C / C composite materials have a series of excellent properties such as low density, high specific strength, high specific modulus, low thermal expansion coefficient, thermal shock resistance and ablation resistance, and have broad application prospects in aviation, aerospace, nuclear energy and civil fields. However, since the C / C composite material begins to oxidize in an aerobic environment above 450°C, the oxidation directly leads to the increase of the pores of the C / C composite material and the decrease of mechanical properties, and as the temperature increases, the degree of oxidation of the composite material It shows a significant upward trend. If effective oxidation protection measures are not taken, the long-term use of C / C ...

Claims

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Application Information

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IPC IPC(8): C04B35/83C04B35/622
Inventor 董志军李轩科张旭黄家骏袁观明丛野
Owner WUHAN UNIV OF SCI & TECH
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