CN113603509A - Preparation method of oxidation-resistant ablation coating on surface of C/C composite material - Google Patents
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Abstract
The invention relates to a preparation method of an anti-oxidation ablation coating on the surface of a C/C composite material. By adopting a chemical liquid phase vaporization deposition process and utilizing the special skin effect, the ultrahigh temperature ceramic precursor is subjected to cracking reaction and gradually deposited on the surface of the C/C composite material. And finally, performing high-temperature heat treatment to fully convert the ultrahigh-temperature ceramic, thereby preparing the oxidation-resistant ablative coating on the surface of the C/C composite material. In the invention, the chemical liquid phase vaporization deposition process parameters, the components and proportion of the ceramic precursor and the high-temperature heat treatment parameters have direct influence on the preparation of the coating, and the microstructure and the tissue components of the surface coating can be regulated and controlled by adjusting the process parameters. The innovation of the invention is that a chemical liquid phase vaporization deposition process is adopted, and the specific skin effect is utilized to prepare the anti-oxidation ablation coating on the surface of the C/C composite material, so that the defects of nonuniform coating thickness, low bonding strength with a matrix, non-uniform ceramic distribution, non-compact structure and the like prepared by the traditional process are overcome, and the further improvement of the anti-oxidation and anti-ablation performances of the coating on the surface of the C/C composite material is realized.
Description
Technical Field
The invention belongs to the technical field of C/C composite material surface coatings, and particularly relates to a preparation process method of a C/C composite material surface oxidation-resistant ablation coating.
Background
With the increasing competition situation of exploring space and earth surface space in various countries, high-temperature thermal structural materials play a more important role in the future aerospace vehicle application. The carbon/carbon (C/C) composite material is used as an advanced high-temperature thermal structure material and has the characteristics of low density, small Coefficient of Thermal Expansion (CTE), no decrease and no reverse increase of mechanical strength along with the temperature increase and the like. Therefore, the composite material has specific contribution in the aspects of improving the body structure of the aircraft, improving the comprehensive performance of the aircraft and the like, and is an important strategic material for developing national defense and military industry and national economy. However, C/C composites begin to oxidize in oxygen-containing environments above 370 ℃, causing damage to the fibers and matrix, limiting their widespread use. Secondly, the material can be subjected to ablation impact caused by high-temperature and high-speed airflow during service, and the service reliability and stability of the material are seriously affected. Therefore, to solve the problem of neck sticking of the C/C composite material in aerospace application, the oxidation resistance and ablation resistance of the C/C composite material in a high-temperature environment must be improved.
At present, one effective method for improving the oxidation and ablation resistance of the C/C composite material is to prepare a protective coating on the surface of the C/C composite material to isolate the C/C composite material from oxygen-containing gas and high-temperature environment. The protective coating composed of the ultrahigh-temperature ceramic has a high melting point, a wider protection temperature range and good high-temperature stability, so that the protective coating is an ideal material for the surface oxidation and ablation resistant coating of the C/C composite material. The commonly used preparation technology of the oxidation-resistant ablative coating mainly comprises an embedding method, a chemical vapor deposition method, an electrophoretic deposition method, a plasma spraying method and the like. However, the coating prepared by the process methods has the problems of uneven thickness, weak bonding force with a substrate, loose structure, more impurities and the like, and the wide application of the coating technology is seriously limited.
Document 1 "X.R. Ren, H.J. Li, K.Z. Li, Q.G. Fu. Oxidation protection of ultra-high temperature ceramic ZrxTa1-xB2-SiC/SiC coating prepared by in-situ reaction method for carbon/carbon composites [J]Journal of European Ceramic Society, 2015, 35 (3): 897-xTa1- xB2-SiC/SiC multiphase ceramic coatings with short production cycle, dense structure and high bond strength to the substrate, thus from room temperature to 1500 deg.foAnd the good oxidation resistance is shown in a wide temperature range of C. Nevertheless, the coating prepared by the embedding method is easy to have the phenomenon of uneven thickness, so that the composite material in the weak area of the coating thickness is seriously oxidized and corroded. Document 2 "A. Mohan, A. Udayakumar, A.S. Gandhi. High temperature oxidation reaction behavor of CVD β -SiC seed coated SiCf/SiC composites in static dry air and combustion environment [J]9472-9480 by chemical vapor deposition, the coating has uniform components and less impurity, thus playing a certain protection role in oxyacetylene combustion atmosphere. However, the coating prepared by the chemical vapor deposition method has a long period and low bonding strength with a substrate, so that a large amount of coating is peeled off from the surface of the composite material during the ablation process, and the oxidation of the composite material is accelerated. Document 3 "J.F. Huang, Q. Yang, T. Yang, L.Y. Cao, Q.F. Zhang. Microtherapy and anti-oxidation property of porous oxidation reactive porous adsorption for SiC-C/C complexes [ J.F. Huang, Q. Yang, T. Yang, L.Y. Cao]Surface and Coatings Technology, 2011, 205 (21-22): 5077- 5082. "the mullite coating is prepared by electrophoretic deposition, and the coating has uniform distribution of components and controllable thickness, thereby showing better oxidation resistance. However, the coating prepared by the electrophoretic deposition method has a loose structure, needs to be densified at a later stage, and has high requirements on the size of ceramic particles, so that the application of the coating is limited. Document 4 "Y.L. Zhang, Z.X. Hu, H.J. Li, J.C. ren. approximation resistance of ZrB2-SiC coating prepared by supersonic atmosphere plasma spraying for SiC-coating carbon/carbon composites [J]Ceramic International, 2014, 40 (9): 14749-2The SiC coating has compact structure, high deposition efficiency and uniform thickness, thereby showing better ablation resistance in an ablation test. However, in the plasma spraying process, raw materials are easily oxidized, so that the content of impurity phases of the prepared coating is high, and the protection effect of the coating is reduced. Therefore, a new preparation method of the oxidation-resistant ablative coating needs to be found at present to overcome the defect that the coating is not oxidized by the oxidation-resistant ablative coatingThe defects of the prior art are compensated.
The idea of the invention is that by adopting a chemical liquid phase vaporization deposition process, and utilizing the characteristics of high deposition rate, controllable components of deposition products, high density, uniform distribution and the like, under the action of a skin effect, the ultrahigh temperature ceramic precursor is cracked and gradually deposited on the surface of the C/C composite material, and finally is subjected to high temperature heat treatment conversion, so that the oxidation resistant ablation coating which has a compact structure, uniform thickness, low impurity phase content, uniform ceramic distribution and high bonding strength with a matrix is prepared in a short time.
Disclosure of Invention
The invention aims to provide a process method for preparing an anti-oxidation ablation coating on the surface of a C/C composite material, which aims to overcome the defects of long preparation period, high content of coating magazine phase, non-uniform thickness, low bonding strength with a matrix, non-uniform ceramic distribution and the like in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
step 1, selecting a C/C composite material as a base material, polishing the surface smoothly by using sand paper, then ultrasonically cleaning by using deionized water, removing impurities, and drying in an oven;
step 2, dissolving an organic ceramic precursor in an organic solvent to prepare an organic ceramic precursor solution;
and 3, placing the C/C composite material in the step 1 into a chemical liquid phase evaporation deposition furnace, and pouring the prepared organic ceramic precursor solution into a reaction container. Then the reaction temperature is raised from room temperature to 1000-oC, after depositing for a period of time, gradually cooling to room temperature, turning off the power supply, and taking out the sample after the sample is cooled;
step 4, placing the prepared sample into a high-temperature tube furnace, and raising the reaction temperature from room temperature to 1500-oAnd C, after keeping the temperature for a period of time, gradually reducing the temperature to room temperature, turning off the power supply, and naturally cooling. In the whole heat treatment process, high-purity argon is always introduced into the tube furnace, and the flow rate of the argon is 40cm3Min, the pressure in the furnace is 1 atm.
The density of the C/C composite material is 1.5-1.8 g/cm3。
The organic ceramic precursor is SiC precursor, TaC precursor and TaB precursor2Precursor, ZrC precursor, ZrB2Precursor, HfC precursor, HfB2One or more of the precursors.
The organic solvent is one of kerosene, cyclohexane, toluene and xylene.
The organic precursor solution consists of 10-30% of organic ceramic precursor and 70-90% of organic solvent by mass percent.
The chemical liquid phase vaporization deposition temperature is 1000-oC, the rate of temperature rise is 10oC/min, and the deposition time is 4-8 h.
The temperature of the high-temperature heat treatment is 1500-oC, the rate of temperature rise is 15oC/min, and the heat preservation time is 1-3 h.
Advantageous effects
The invention provides a process method for preparing an anti-oxidation ablative coating on the surface of a C/C composite material, which comprises the steps of cracking and gradually depositing an ultrahigh-temperature ceramic precursor on the surface of the C/C composite material by adopting a chemical liquid phase vaporization deposition process and utilizing the specific skin effect of the chemical liquid phase vaporization deposition process, and finally performing high-temperature heat treatment to prepare the anti-oxidation ablative coating. The chemical liquid phase vaporization deposition process has the characteristics of high preparation efficiency, controllable components of deposition products, high density, uniform distribution and the like, so that the high-temperature protective coating which has a compact structure, uniform thickness, low impurity phase content, uniform ceramic distribution and high bonding strength with a matrix can be prepared in a short time. Therefore, the invention has considerable development prospect and obvious economic and social benefits.
Compared with the background technology, the invention overcomes the defects of the prior common coating preparation technology, such as uneven coating thickness, long preparation period, weak bonding force with a substrate, loose coating structure, uneven component distribution and high impurity phase content, thereby having obvious advantages. In addition, the preparation method provided by the invention is simple and reasonable in process, convenient to operate, high in efficiency, safe and reliable. Taking the example of preparing the ZrC coating on the surface of the C/C composite material by the chemical liquid phase vapor deposition process, the thickness of the ZrC coating prepared within 10 hours by the process is about 120 mu m, and the ZrC coating is uniform in thickness and compact in microstructure. Therefore, the chemical liquid phase vaporization deposition process can greatly shorten the preparation period of the coating and realize large-scale high-efficiency production, and is an ideal process method for preparing the surface protective coating.
Drawings
FIG. 1 is a flow chart of preparing an anti-oxidation ablative coating on the surface of a C/C composite material by a chemical liquid phase vapor deposition process.
FIG. 2 is a view showing an apparatus of a chemical liquid phase vapor deposition furnace.
FIG. 3 is a BSE diagram of a ZrC coating on the surface of the C/C composite material prepared in example 1.
FIG. 4 is the XRD pattern of the ZrC coating on the surface of the C/C composite material prepared in example 1.
Detailed Description
Example 1:
(1) the density is 1.70g/cm3The C/C composite material of (1) was processed into a cylindrical shape having a size of phi 80mm x 20mm, and the surface was polished smooth with sandpaper. Then ultrasonically cleaning in deionized water for 3 times, 10min each time, and placing into a container 85oC, drying in an oven for 12 hours;
(2) weighing 600g of ZrC precursor and 6L of dimethylbenzene, and dissolving the ZrC precursor in the dimethylbenzene to obtain a ZrC precursor solution;
(3) placing the dried C/C composite material in a chemical liquid phase evaporation deposition furnace, pouring the prepared ZrC precursor solution into a reaction container, and then pouring 10 parts of the ZrC precursor solution into the reaction containeroThe temperature rise speed of C/min is increased from room temperature to 1100oC, depositing for 6 h, and then 10 hoThe cooling rate of C/min is 1100oC, gradually cooling to room temperature, turning off a power supply, cooling the sample along with the furnace, and finally taking out the sample;
(4) placing the sample in the step 3 into a high-temperature tube furnace for heat treatment, and firstly, 15 parts of the sample is placedoThe temperature rise speed of C/min is increased from room temperature to 1700oC, after heat preservation for 3 hours, further adding 20 hoursoAnd (4) reducing the temperature of the sample to room temperature from 1700 ℃, turning off a power supply, and cooling the sample along with the furnace. The wholeIn the heat treatment process, argon with the purity of 99.99 percent is always introduced into the tube furnace, and the flow rate of the argon is controlled to be 40cm3Min, the pressure in the furnace is 1 atm. And cooling the sample to room temperature to prepare the C/C composite material with the ZrC coating deposited on the surface.
Example two:
(1) the density is 1.80g/cm3The C/C composite material of (1) was processed into a cylindrical shape having a size of phi 80mm x 15 mm, and the surface was polished smooth with sandpaper. Then ultrasonically cleaning in deionized water for 3 times, 10min each time, and placing into a container 85oC, drying in an oven for 12 hours;
(2) weighing 1000 g of HfB2Precursor and 7L xylene, reaction of HfB2Dissolving the precursor in xylene to obtain HfB2Precursor solution;
(3) placing the dried C/C composite material in a chemical liquid phase evaporation deposition furnace, and preparing HfB2The precursor solution is poured into a reaction vessel and subsequently at 10oThe temperature rise speed of C/min is increased from room temperature to 1200oC, depositing for 4 h, and then performing deposition for 10 hoThe cooling rate of C/min is from 1200oC, gradually cooling to room temperature, turning off a power supply, cooling the sample along with the furnace, and finally taking out the sample;
(4) placing the sample in the step 3 into a high-temperature tube furnace for heat treatment, and firstly, 15 parts of the sample is placedoThe temperature rise speed of C/min is increased from room temperature to 1800oC, after heat preservation for 2 hours, adding 20 percent of the mixtureoAnd (4) reducing the temperature reduction speed of C/min from 1800 ℃ to room temperature, turning off a power supply, and cooling the sample along with the furnace. In the whole heat treatment process, argon with the purity of 99.99 percent is always introduced into the tube furnace, and the flow rate of the argon is controlled to be 40cm3Min, the pressure in the furnace is 1 atm. After the sample is cooled to room temperature, HfB deposited on the surface is prepared2Coated C/C composite materials.
Example three:
(1) the density is 1.60 g/cm3The C/C composite material of (1) was processed into a cylindrical shape having a size of phi 80mm x 10 mm, and the surface was polished smooth with sandpaper. Then ultrasonically cleaning in deionized water for 3 times, 10min each time, and placing into a container 85oC, drying in an oven for 12 hours;
(2) weighing 1500 g of TaC precursor and 7L of dimethylbenzene, and dissolving the TaC precursor in the dimethylbenzene to obtain a TaC precursor solution;
(3) placing the dried C/C composite material in a chemical liquid phase evaporation deposition furnace, pouring the prepared TaC precursor solution into a reaction container, and then pouring 10 percent of the prepared TaC precursor solution into the reaction containeroThe temperature rise speed of C/min is increased from room temperature to 1000oC, depositing for 5 h, and then performing deposition for 10 hoThe cooling rate of C/min is 1000oC, gradually cooling to room temperature, turning off a power supply, cooling the sample along with the furnace, and finally taking out the sample;
(4) placing the sample in the step 3 into a high-temperature tube furnace for heat treatment, and firstly, 15 parts of the sample is placedoThe temperature rise speed of C/min is increased from room temperature to 1600oC, after heat preservation for 3 hours, further adding 20 hoursoAnd (4) reducing the temperature reduction speed of C/min from 1600 ℃ to room temperature, turning off a power supply, and cooling the sample along with the furnace. In the whole heat treatment process, argon with the purity of 99.99 percent is always introduced into the tube furnace, and the flow rate of the argon is controlled to be 40cm3Min, the pressure in the furnace is 1 atm. And cooling the sample to room temperature to prepare the C/C composite material with the TaC coating deposited on the surface.
Example four:
(1) the density is 1.75 g/cm3The C/C composite material of (1) was processed into a cylindrical shape having a size of phi 80mm x 20mm, and the surface was polished smooth with sandpaper. Then ultrasonically cleaning in deionized water for 3 times, 10min each time, and placing into a container 85oC, drying in an oven for 12 hours;
(2) weighing 1000 g of SiC precursor and 6L of dimethylbenzene, and dissolving the SiC precursor in the dimethylbenzene to obtain a SiC precursor solution;
(3) placing the dried C/C composite material in a chemical liquid phase evaporation deposition furnace, pouring the prepared SiC precursor solution into a reaction container, and then pouring the prepared SiC precursor solution into the reaction container by 10 degreesoThe temperature rise speed of C/min is increased from room temperature to 1200oC, depositing for 4 h, and then performing deposition for 10 hoThe cooling rate of C/min is from 1200oC, gradually cooling to room temperature, turning off a power supply, cooling the sample along with the furnace, and finally taking out the sample;
(4) placing the sample in the step 3 into a high-temperature tube furnace for heat treatment, and firstly, 15 parts of the sample is placed oThe temperature rise speed of C/min is increased from room temperature to 1700oC, after heat preservation for 2 hours, adding 20 percent of the mixtureoAnd (4) reducing the temperature of the sample to room temperature from 1700 ℃, turning off a power supply, and cooling the sample along with the furnace. In the whole heat treatment process, argon with the purity of 99.99 percent is always introduced into the tube furnace, and the flow rate of the argon is controlled to be 40cm3Min, the pressure in the furnace is 1 atm. And cooling the sample to room temperature to prepare the C/C composite material with the SiC coating deposited on the surface.
Claims (7)
1. A preparation method of an oxidation-resistant ablation coating on the surface of a C/C composite material is characterized by comprising the following steps: the method comprises the following steps:
step 1, selecting a C/C composite material as a base material, polishing the surface smoothly by using sand paper, then ultrasonically cleaning by using deionized water, removing impurities, and drying in an oven;
step 2, dissolving an organic ceramic precursor in an organic solvent to prepare an organic ceramic precursor solution;
step 3, placing the C/C composite material in the step 1 into a chemical liquid phase evaporation deposition furnace, pouring the prepared organic ceramic precursor solution into a reaction container, and then raising the reaction temperature from room temperature to 1000-oC, after depositing for a period of time, gradually cooling to room temperature, turning off the power supply, and taking out the sample after the sample is cooled;
step 4, placing the prepared sample into a high-temperature tube furnace, and raising the reaction temperature from room temperature to 1500-oC, after preserving heat for a period of time, gradually reducing the temperature to room temperature, turning off a power supply, naturally cooling, and in the whole heat treatment process, introducing high-purity argon into the tubular furnace all the time, wherein the flow rate of the argon is 40cm3Min, the pressure in the furnace is 1 atm.
2. The preparation process method of the C/C composite material surface oxidation and ablation resistant coating according to claim 1, characterized in that: the density of the C/C composite material is 1.50-1.80g/cm3。
3. The C/C composite surface oxidation and ablation resistant coating according to claim 1The preparation process method is characterized by comprising the following steps: the organic ceramic precursor is SiC precursor, TaC precursor and TaB precursor2Precursor, ZrC precursor, ZrB2Precursor, HfC precursor, HfB2One or more of the precursors.
4. The preparation process method of the C/C composite material surface oxidation and ablation resistant coating according to claim 1, characterized in that: the organic solvent is one of kerosene, cyclohexane, toluene and xylene.
5. The preparation process method of the C/C composite material surface oxidation and ablation resistant coating according to claim 1, characterized in that: the organic precursor solution consists of 10-30% of organic ceramic precursor and 70-90% of organic solvent by mass percent.
6. The preparation process method of the C/C composite material surface oxidation and ablation resistant coating according to claim 1, characterized in that: the chemical liquid phase vaporization deposition temperature is 1000-oC, the rate of temperature rise is 10oC/min, and the deposition time is 4-8 h.
7. The preparation process method of the C/C composite material surface oxidation and ablation resistant coating according to claim 1, characterized in that: the temperature of the high-temperature heat treatment is 1500-oC, the rate of temperature rise is 15oC/min, and the heat preservation time is 1-3 h.
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| CN114436680A (en) * | 2022-03-02 | 2022-05-06 | 成都理工大学 | Preparation process method of mineral material and ultrahigh-temperature ceramic synergistically modified C/C composite material |
| CN115650752A (en) * | 2022-10-17 | 2023-01-31 | 航天特种材料及工艺技术研究所 | Preparation method of ultrahigh-temperature ceramic modified SiC/SiC composite material |
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| CN114436680A (en) * | 2022-03-02 | 2022-05-06 | 成都理工大学 | Preparation process method of mineral material and ultrahigh-temperature ceramic synergistically modified C/C composite material |
| CN115650752A (en) * | 2022-10-17 | 2023-01-31 | 航天特种材料及工艺技术研究所 | Preparation method of ultrahigh-temperature ceramic modified SiC/SiC composite material |
| CN115650752B (en) * | 2022-10-17 | 2024-01-16 | 航天特种材料及工艺技术研究所 | Preparation method of ultra-high temperature ceramic modified SiC/SiC composite material |
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