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CN-116427034-B - Carbonaceous material with coating and preparation method thereof

CN116427034BCN 116427034 BCN116427034 BCN 116427034BCN-116427034-B

Abstract

The invention discloses a carbonaceous material with a coating and a preparation method thereof, wherein the carbonaceous material is prepared by the following steps of (1) forming a microstructure groove on the surface of a matrix and preparing a metal catalyst layer, (2) impregnating the matrix by using silicon-containing slurry, (3) heating and growing the matrix of the carbonaceous material to form a silicon carbide nanowire connecting layer to obtain an intermediate product A, (4) depositing and forming a silicon carbide nanowire reinforced silicon carbide layer on the intermediate product A to obtain an intermediate product B, (5) depositing and preparing a silicon carbide-zirconium carbide composite layer on the intermediate product B, and then carrying out post treatment to obtain an intermediate product C, and (6) depositing and preparing a zirconium carbide layer on the intermediate product C. The invention avoids the problems of single coating in the prior art, ensures the transition and bonding strength between the coating and the matrix, promotes the coating and the matrix to present a three-dimensional alternate mechanical matching structure, and effectively improves the bonding strength of the interface between the coating and the matrix through mechanical bridging and interface constraint.

Inventors

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Assignees

  • 湖南泰坦未来科技有限公司

Dates

Publication Date
20260512
Application Date
20230329

Claims (5)

  1. 1. A method for preparing a coated carbonaceous material, comprising the steps of: (1) Forming a microstructure groove on the surface of a carbonaceous material matrix, and preparing a metal catalyst layer on the surface of the carbonaceous material matrix, wherein the depth of the microstructure groove is 10-20 mu m, and the width of the microstructure groove is 2-5 mu m; (2) Impregnating the carbonaceous material matrix by using a silicon-containing slurry, wherein the silicon-containing slurry comprises 10 parts by mass of nano silicon powder and 2-3 parts by mass of waxy carbon source; (3) Heating and growing the impregnated carbonaceous material matrix in a reaction device to form a silicon carbide nanowire connection layer to obtain an intermediate product A, heating and growing the silicon carbide nanowire connection layer for 1-2 hours under vacuum, then introducing diluent gas, silicon source gas and carbon source gas into the reaction device to continue growing for 0.5-2 hours, wherein the growth temperature of the silicon carbide nanowire connection layer is 1100-1350 ℃, the growth time is 1.5-4 hours, the volume ratio of the carbon source gas to the silicon source gas is 1 (2-4), and the volume of the diluent gas is 3-5 times of the total volume of the carbon source gas and the silicon source gas; (4) Placing the intermediate product A in a deposition device, introducing diluent gas, silicon source gas and carbon source gas, and depositing on the intermediate product A to form a silicon carbide nanowire reinforced silicon carbide layer to obtain an intermediate product B; (5) Depositing and preparing a silicon carbide-zirconium carbide composite layer on the intermediate product B, and performing post-treatment to obtain an intermediate product C, wherein the silicon carbide-zirconium carbide composite layer is deposited and obtained by adopting a double-gas-phase communication method, the introduced gas is silicon tetrachloride, zirconium tetrachloride, carbon source gas and diluent gas, and the molar ratio of the silicon tetrachloride to the zirconium tetrachloride is 1:1; (6) And depositing and preparing a zirconium carbide layer on the intermediate product C to obtain the carbonaceous material with the coating.
  2. 2. The method for preparing the coated carbonaceous material according to claim 1, wherein the impregnating treatment in the step (2) is performed by brushing the silicon-containing slurry on the surface of the carbonaceous material substrate and rotationally impregnating the carbonaceous material substrate at room temperature, wherein the brushing times are 3-5 times, the drying is performed at room temperature for 2-10 min after each brushing, the impregnating time is 1-3 h, and the rotational speed is 10-30/turn.
  3. 3. The method for preparing a coated carbonaceous material according to claim 1, wherein the deposition temperature of the silicon carbide nanowire reinforced silicon carbide layer in the step (4) is 1000-1400 ℃ and the deposition time is 5-20 hours.
  4. 4. The method for preparing a coated carbonaceous material according to any one of claims 1 to 3, wherein the zirconium carbide layer in step (6) is prepared by a high temperature chemical vapor deposition method, the deposition temperature is 1700 to 1800 ℃, the deposition time is 3 to 5 hours, the raw material gas is zirconium tetrachloride, the diluent gas is hydrogen, and the volume ratio of the raw material gas to the diluent gas is 1:1.
  5. 5. A coated carbonaceous material produced by the production process according to any one of claims 1 to 4.

Description

Carbonaceous material with coating and preparation method thereof Technical Field The invention relates to the technical field of coating preparation of carbonaceous materials, in particular to a carbonaceous material with a coating and a preparation method thereof. Background The graphite has excellent electric conductivity and heat conductivity, small thermal expansion coefficient and excellent thermal shock resistance due to the porosity, and small resistance temperature coefficient and thermal inertia, can be rapidly heated and cooled, and has small heat loss. Graphite is commonly used as a heating element, a heat preservation cylinder, a guide cylinder, a crucible and the like in a special industrial furnace. With the comprehensive development of the semiconductor industry, when materials such as single crystal silicon, groan grafting, indium phosphide and the like are extracted and a heating furnace for wafer growth selects graphite as a heating body, a heat preservation cylinder, a guide cylinder and a crucible, the graphite material can not meet the requirement of extracting high-purity materials due to the defects of the graphite material. Because, first, when graphite materials are used as certain furnace-type heating elements, cracks are generated at the junction of the cold end and the hot end due to the temperature difference between the cold end and the hot end. Because of the special airtight structure of the vacuum furnace, the damaged graphite resistance heating element cannot be replaced in a high-temperature state, the vacuum furnace can only work continuously under the condition of incomplete heating element, and the heating effect of the vacuum furnace and the temperature in the furnace cannot be guaranteed. And secondly, the graphite material has lower strength and large brittleness, and has larger processing and transportation difficulties. In the process of refining high-capacity semiconductor materials, the graphite crucible cannot bear the load of the high-capacity semiconductor materials, and the current advanced mass production process is seriously affected. In addition, the graphite material is continuously volatilized at high temperature, so that two negative effects are brought to the fact that firstly, carbon atoms are diffused into a wafer to cause the quality of the wafer to be reduced, and secondly, a large number of corrosion pits are formed on the surface of the graphite, and the service life is reduced. Due to the use defects of the graphite material, the scales of material industries such as single crystal silicon, groan grafting, indium phosphide and the like and wafer industries are greatly enlarged, and in the solar photovoltaic industry and the semiconductor industry, the improvement of material quality and the reduction of cost become key for industrial development, and the service time of thermal field materials is urgently required to be prolonged. At present, the C/C composite material has similar resistivity to graphite as a high-temperature composite material which can be used for high temperature up to 2800 ℃, so if the C/C composite material is used as a resistance heating element, a crucible, a guide cylinder, a heat preservation cylinder and the like, stress fracture at the junction of the cold end and the hot end caused by the temperature difference of the cold end and the hot end of the graphite heating element can be effectively relieved, and according to the characteristics of the C/C composite material, a large thin-wall heating element can be manufactured, and the volume of a hearth can be effectively utilized. However, in the field of semiconductors with special purity requirements, when a single C/C composite material is adopted as a material of devices such as a heating body, a heat-preserving cylinder, a crucible, a guide cylinder and the like, carbon atoms are inevitably volatilized, and a new challenge is initiated to the purity requirements of the material; secondly, when the silicon single crystal is used for drawing single crystal silicon, high-temperature silicon steam reacts with a quartz crucible to generate oxidizing substances such as SiO and the like to corrode the outer surfaces of a guide cylinder, a crucible, a heat preservation cylinder and the like, so that the use effect of the guide cylinder is affected, the service life of the guide cylinder is shortened and the like. At present, as an aerospace coating material, a new material of the nano silicon carbide coating has the advantages of high heat conductivity, small thermal expansion coefficient, small carbon diffusion coefficient, stable chemical property, good wear resistance, high temperature resistance, thermal shock resistance, creep resistance and oxidation resistance. In the aerospace field, silicon carbide coatings have been used as high temperature coatings for carbon materials and carbon/carbon composites, which resist gas flows of 2500-3000 ℃ and exhibit excellent oxi