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Preparation method of multicomponent complex carbide coating

A multi-component composite and carbide technology, applied in coatings, metal material coating processes, gaseous chemical plating, etc., can solve problems such as poor oxidation resistance, achieve excellent stability, accurate stoichiometric ratio, and ultra-high temperature resistance. Excellent ablative performance

Active Publication Date: 2019-07-05
NO 59 RES INST OF CHINA ORDNANCE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the C / C composite material has poor oxidation resistance, so it is necessary to modify the C / C composite material or prepare a protective coating on the surface.

Method used

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  • Preparation method of multicomponent complex carbide coating
  • Preparation method of multicomponent complex carbide coating
  • Preparation method of multicomponent complex carbide coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A method for preparing a multi-component composite carbide coating, comprising the following steps in sequence, wherein, for the specific structure of the chemical vapor deposition system used, refer to the attached figure 1 :

[0032] (1) In an argon protective glove box, put TaCl 5 , HfCl 4 and ZrCl 4 Mix the powder and fill it into an alumina crucible; where TaCl 5 , HfCl 4 and ZrCl 4 Prepared at 55%, 35% and 10% respectively by mass percentage;

[0033] (2) Place the substrate sample on the support of the deposition furnace, and feed argon gas with a flow rate of 200ml / min into the deposition furnace for 30 minutes to remove the air in the furnace; then heat the deposition furnace at a heating rate of 5-20°C / min Reach a deposition temperature of 1300°C;

[0034] (3) will contain TaCl 5 , HfCl 4 and ZrCl 4 The crucible of mixed powder is placed on the lifting support in the low temperature zone of the dual temperature zone gasifier, and the lifting support is...

Embodiment 2

[0039] A method for preparing a multi-component composite carbide coating, comprising the following steps in turn, wherein the structure of the chemical vapor deposition system used is the same as in Example 1:

[0040] (1) In an argon protective glove box, put TaCl 5 , HfCl 4 and ZrCl 4 Mix the powder and fill it into an alumina crucible; where TaCl 5 , HfCl 4 and ZrCl 4 Prepared by mass percentage as 75%, 20% and 5% respectively;

[0041] (2) Place the substrate sample on the support of the deposition furnace, and feed argon gas with a flow rate of 200ml / min into the deposition furnace for 30 minutes to remove the air in the furnace; then heat the deposition furnace at a heating rate of 5-20°C / min Reach a deposition temperature of 1400°C;

[0042] (3) will contain TaCl 5 , HfCl 4 and ZrCl 4 The crucible of mixed powder is placed on the lifting support in the low temperature zone of the dual temperature zone gasifier, and the lifting support is raised so that the mou...

Embodiment 3

[0047] A method for preparing a multi-component composite carbide coating, comprising the following steps in turn, wherein the structure of the chemical vapor deposition system used is the same as in Example 1:

[0048] (1) In an argon protective glove box, put TaCl 5 , HfCl 4 and ZrCl 4 Mix the powder and fill it into an alumina crucible; where TaCl 5 , HfCl 4 and ZrCl 4 Prepared as 60%, 30% and 10% respectively by mass percentage;

[0049] (2) Place the substrate sample on the support of the deposition furnace, and feed argon gas with a flow rate of 200ml / min into the deposition furnace for 30 minutes to remove the air in the furnace; then heat the deposition furnace at a heating rate of 5-20°C / min Reach a deposition temperature of 1400°C;

[0050] (3) will contain TaCl 5 , HfCl 4 and ZrCl 4 The crucible of mixed powder is placed on the lifting support in the low temperature zone of the dual temperature zone gasifier, and the lifting support is raised so that the mo...

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Abstract

The invention relates to a preparation method of a multicomponent complex carbide coating. The preparation method sequentially includes the steps that (1) TaCl5, HfCl4 and ZrCl4 mixed powder is put ina crucible under the inert atmosphere; (2) a base sample is placed on a support of a deposition furnace, argon gas is fed into the deposition furnace, and the deposition furnace is heated to the deposition temperature; (3) the crucible containing the mixed powder is put onto a lifting support of a low temperature zone in a dual-temperature zone gasification furnace, the opening of the crucible communicates with a high temperature zone, the heating temperature of the low temperature zone and the heating temperature of the high temperature zone are set, and heating is conducted to completely gasify the mixed powder; and (4) H2 and CH4 are fed into the deposition furnace, mixed gas after complete gasification is fed into the deposition furnace with carrier gas, and the deposition is carriedout under normal pressure. According to the preparation method, the multicomponent complex coating with accurate composition stoichiometric ratios can be obtained, and it can be ensured that the combination of the coating and substrate materials is tight and firm and the stability is excellent.

Description

technical field [0001] The invention relates to the technical field of surface heat protection coatings, in particular to the super high temperature protection of C / C composite materials and graphite and other materials, and in particular to a preparation method of a multi-component composite carbide coating. Background technique [0002] C / C composite material refers to a pure carbon multiphase structure composed of carbon fiber or its fabric as the reinforcing phase, and chemical vapor infiltration pyrolytic carbon or liquid phase impregnated-carbonized resin carbon and pitch carbon as the matrix. C / C composite materials have excellent high-temperature mechanical properties and good thermal shock resistance, and are the main sublimation-type ablation heat-resistant materials and materials with high emissivity. They are widely used in solid rocket engine throat linings and aerospace vehicles. High temperature hot end parts such as nose cones and fairings. However, C / C comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C16/44C23C16/30
CPCC23C16/44C23C16/32
Inventor 李忠盛吴护林丛大龙何庆兵陈大军赵子鹏田武强
Owner NO 59 RES INST OF CHINA ORDNANCE IND