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Preparation method of in-situ synthesized carbon nano-tube modified SiCN ceramic matrix composite material

A technology of carbon nanotube modification and silicon carbon nitrogen ceramics, which is applied in the field of preparation of in-situ self-generated carbon nanotube modified silicon carbon nitrogen ceramic matrix composite materials, can solve the problem that CNTs and SiCN ceramic matrix cannot be generated simultaneously, and achieve The effect of short preparation cycle, realization of integration and simple process

Active Publication Date: 2014-08-20
NORTHWESTERN POLYTECHNICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to overcome the deficiency that CNTs and SiCN ceramic matrix cannot be synchronously generated in the existing CVD / CVI method, the present invention provides a preparation method of in-situ self-generated carbon nanotube modified silicon-carbon-nitrogen ceramic matrix composite material

Method used

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  • Preparation method of in-situ synthesized carbon nano-tube modified SiCN ceramic matrix composite material
  • Preparation method of in-situ synthesized carbon nano-tube modified SiCN ceramic matrix composite material
  • Preparation method of in-situ synthesized carbon nano-tube modified SiCN ceramic matrix composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0025] (1) Select porous Si with an open porosity of 50% 3 N 4 Ceramic substrate (22.86×10.16×2.00mm 3 ) as the base material.

[0026] (2) Using the vacuum impregnation process (vacuuming for 5 minutes, impregnating for 30 minutes), the mass fraction of 1.5wt.% Fe(NO 3 ) 3 9H 2 O acetone solution introduced porous Si 3 N 4 Porcelain interior, then air dry.

[0027] (3) The catalyst Fe(NO 3 ) 3 9H 2 O porous Si in acetone solution 3 N 4 Ceramic substrate and porous Si not treated by step (2) 3 N 4 The ceramic substrate is suspended on the supporting sample holder in the CVD / CVI SiCN vacuum reaction furnace at the same time, and the two groups of samples are located in the center of the isothermal zone in the furnace. Using CVD / CVI process on two groups of different porous Si 3 N 4 SiCN with uniform thickness is deposited on the ceramic, and the reaction precursor is SiCl 4 -CH 4 -NH 3 -H 2 -Ar(SiCl 4 、CH 4 with NH 3 The flow ratio is 6:5:2), the reaction...

Embodiment 2

[0037] (1) Select porous Al with an open porosity of 15% 2 o 3 Ceramic substrate (22.86×10.16×2.00mm 3 ) as the base material.

[0038] (2) Ni(NO 3 ) 2 ·6H 2 O ethanol solution introduces porous Al 2 o 3 Porcelain interior, then air dry.

[0039] (3) The catalyst Ni(NO 3 ) 2 ·6H 2 Porous Al in O ethanol solution 2 o 3 The ceramic substrate is suspended on the supporting sample holder in the CVD / CVI SiCN vacuum reaction furnace, and the sample is in the center of the isothermal zone in the furnace. Porous Al by CVD / CVI process 2 o3 SiCN with uniform thickness is deposited on the ceramic, and the reaction precursor is SiCl 4 -C 3 h 6 -NH 3 -H 2 -Ar(SiCl 4 、C 3 h 6 with NH 3 The flow ratio is 6:5:2), the reaction temperature is 700°C, the reaction time is 10 hours, and the furnace pressure is 400Pa.

[0040] Due to the catalyst Ni(NO 3 ) 2 ·6H 2 The Ni nanoparticles transformed from O will easily capture a large number of free carbon atoms in the Si-C-N ...

Embodiment 3

[0042] (1) Select a 2D carbon fiber prefabricated body with an open porosity of 50% (the plane size is 50×50mm 2 ) as the base material.

[0043] (2) Using the vacuum impregnation process (vacuuming for 10 minutes, impregnating for 40 minutes), the mass fraction of 2.0wt.% Fe(NO 3 ) 3 9H 2 O acetone solution was introduced into the interior of the 2D carbon fiber preform, followed by air drying.

[0044] (3) The catalyst Fe(NO 3 ) 3 9H 2 The 2D carbon fiber prefabricated body of O acetone solution is suspended on the supporting sample holder in the CVD / CVISiCN vacuum reaction furnace, and the sample is located in the center of the isothermal zone in the furnace. Using CVD / CVI process to deposit SiCN with uniform thickness on 2D carbon fiber preform, the reaction precursor is CH 3 SiCl 3 -CH 4 -NH 3 -H 2 -Ar(CH 3 SiCl 3 、CH 4 with NH 3 The flow ratio is 6:5:2), the reaction temperature is 1000°C, the reaction time is 40 hours, and the furnace pressure is 1KPa.

...

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Abstract

The invention discloses a preparation method of an in-situ synthesized carbon nano-tube modified SiCN ceramic matrix composite material so as to solve the technical problem that CNTs (carbon nano-tubes) and an SiCN ceramic matrix cannot be generated synchronously in existing CVD / CVI (chemical vapor deposition / chemical vapor infiltration) methods. According to the technical scheme involved in the invention, a CVD / CVI process is adopted, respectively, SiCl4, SiHCl3 or CH3SiCl3 is taken as a silicon source, CH4 or C3H6 is taken as a carbon source, NH3 is taken as a nitrogen source, H2 is employed as a bubbling carrier gas and reducing gas, and Ar is adopted as a diluent gas. By adding Fe(NO3)3.9H2O, Co(NO3)2.6H2O or Ni(NO3)2.6H2O and other metal salt catalysts, the Fe, Co, Ni nanoparticles produced by metal salt reduction can be utilized to capture a large number of free carbon atoms existing in the Si-C-N system, so that the purpose of synchronous synthesis of CNTs and the SiCN ceramic matrix on a base material can further be achieved.

Description

technical field [0001] The invention relates to a method for preparing a silicon-carbon-nitrogen ceramic-based composite material, in particular to a method for preparing an in-situ self-generated carbon nanotube modified silicon-carbon-nitrogen ceramic-based composite material. Background technique [0002] As an important high-temperature structural / functional integrated material, SiCN ceramics not only have high strength, high hardness, excellent thermal conductivity and thermal stability, but also have excellent microwave absorption properties, so they are widely used in aviation and aerospace. In the field of high temperature absorbing thermal structural parts. However, the inherent brittleness of SiCN ceramics greatly limits its applicability in some harsh environments. Due to the extraordinary mechanical properties of CNTs (Young's modulus reached 1.3TPa), many researchers have begun to improve the fracture toughness of materials by introducing CNTs into the ceramic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/78C04B35/622C04B35/515
Inventor 殷小玮郝轩成来飞张立同
Owner NORTHWESTERN POLYTECHNICAL UNIV
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