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Preparation method of carbon material surface boride solid solution modified silicon-based coating

A technology of carbon materials and solid solutions, which is applied in the field of preparation of boride solid solution modified silicon-based coatings on the surface of carbon materials, can solve the problem of difficult control of the solid solubility content of the ultra-high temperature ceramic boride solid solution phase of the coating thickness, and achieve improvement effect of density

Active Publication Date: 2018-06-29
CHINA UNIV OF MINING & TECH
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Problems solved by technology

[0014] The purpose of the present invention is to provide a method for preparing a boride solid solution modified silicon-based coating on the surface of a carbon material to solve the problem of preparing NB on the surface of an existing carbon material. 2 -SiC(N=Zr x Ta 1-x , Hf x Ta 1-x or Zr x Hf 1-x , x=0~1) coating thickness, solid solubility of ultra-high temperature ceramic boride solid solution phase and its content in the coating are not easy to control in the coating method

Method used

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preparation example Construction

[0032] The preparation method of anti-oxidation coating, first configure the ultra-high temperature ceramic boride solid solution NB with controllable content 2 Modified silicon-based composite ceramic slurry, wherein N=Zr x Ta 1-x , Hf x Ta 1-x or Zr x f 1-x , x=0~1, followed by brushing, dipping or spraying ultra-high temperature ceramic boride solid solution NB on the surface of carbon material substrate with SiC inner coating 2 The preset layer of the slurry, after the preset layer is obtained, is sintered and combined by ultra-high temperature heat treatment to form a coating.

[0033] The specific steps are:

[0034] Step 1: Grinding the carbon material with sandpaper of different roughness, followed by ultrasonic cleaning and drying, the carbon material is graphite or C / C composite material;

[0035] Step 2: Prepare the SiC inner coating: uniformly mix the C powder with a mass fraction of 10-30% and the Si powder with 70-90% and dry it, and then dry the carbon ma...

Embodiment 1

[0044] Step 1: Ultrasonic cleaning and drying of graphite after sanding with different roughnesses.

[0045] Step 2: Prepare the SiC inner coating: evenly mix Si powder with a mass fraction of 75% and C powder with 25% and dry it, then put the graphite treated in step 1 into a graphite crucible and use the dried powder Then put the graphite crucible with powder and graphite into the ultra-high temperature heat treatment furnace, pass it into the argon atmosphere for protection, and raise the temperature of the ultra-high temperature heat treatment furnace to 2000 °C at a heating rate of 10 °C / min, keep it for 3 hours, and then The graphite surface gets a SiC inner coating.

[0046] Step 3: Preparation of Zr 0.5 Ta 0.5 B 2 -SiC outer coating: Zr 0.5 Ta 0.5 B 2Powder (70wt.%), SiC powder (15wt.%), Si powder (10wt.%) and C powder (5wt.%) are evenly mixed and dried, then add a certain amount of silica sol (the volume of silica sol is mixed with The ratio of powder mass is 1...

Embodiment 2

[0050] Step 1: Ultrasonic cleaning and drying of graphite after sanding with different roughnesses.

[0051] Step 2: Prepare the SiC inner coating: evenly mix Si powder with a mass fraction of 80% and C powder with 20% and dry it, then put the graphite treated in step 1 into a graphite crucible and use the dried powder Then put the graphite crucible with powder and graphite into the ultra-high temperature heat treatment furnace, pass it into the argon atmosphere for protection, and raise the temperature of the ultra-high temperature heat treatment furnace to 2100 °C at a heating rate of 15 °C / min, keep it for 2 hours, and then The graphite surface gets a SiC inner coating.

[0052] Step 3: Preparation of Hf 0.8 Ta 0.2 B 2 -SiC outer coating: Hf 0.8 Ta 0.2 B 2 Powder (20wt.%), SiC powder (60wt.%), Si powder (15wt.%) and C powder (5wt.%) are evenly mixed and dried, then add a certain amount of silica sol (the volume of silica sol is mixed with The powder mass ratio is 2ml...

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Abstract

The invention discloses a preparation method of a carbon material surface boride solid solution modified silicon-based coating, and belongs to a preparation method of a carbon material surface anti-oxidation coating. The preparation method comprises the following steps: preparing content-controllable boride solid solution NB2 modified silicon-based composite ceramic slurry, wherein N is equal to ZrxTa1-x, HfxTa1-x or ZrxHf1-x, and x is equal to 0-1; applying a preset layer of the NB2 slurry, by brushing, dip coating or spraying, to the surface of a carbon material matrix with a SiC internal coating; performing heat treatment and sintering to synthesizing the coating. According to the preparation method disclosed by the invention, the solid solubility of the solid solution phase in the coating is controlled by taking boride solid solution powder as a raw material; the component content of the coating can be controlled by controlling and designing the slurry-powder ratio of composite ceramic; control on the coating thickness can be realized through control on the times of the brushing, dip coating or spraying. Through late heat treatment on the preset layer, the density of the coating and the bonding strength of the internal coating interface can be enhanced. The preparation method disclosed by the invention has the advantages of simple preparation technology, dense and uniform coating and relatively low production cost, and is suitable for carbon material components different in shape and size.

Description

technical field [0001] The invention relates to a method for preparing an anti-oxidation coating on the surface of a carbon material, in particular to a method for preparing a boride solid solution modified silicon-based coating on the surface of a carbon material. Background technique [0002] Carbon materials (graphite, C / C composite materials) are a class of excellent high-temperature structural materials, which have the advantages of high strength, high temperature resistance, small specific gravity, high thermal conductivity and low expansion coefficient, and can withstand extremely high heating in ultra-high temperature environments The effect of rate on its performance can be maintained at high temperatures above 2000°C, and it is widely used in the aerospace field. [0003] Since the carbon material is an all-carbon material, as the temperature gradually increases, its strength shows a gradual increase trend. Although it has excellent mechanical properties at high te...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B41/89
CPCC04B41/52C04B41/89C04B2235/9684C04B41/4545C04B41/455C04B41/5059C04B41/507
Inventor 任宣儒李贺军冯培忠郭立童张平鞠治成
Owner CHINA UNIV OF MINING & TECH
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