CN107915499B - Method for repairing C/SiC ceramic matrix composite - Google Patents
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- CN107915499B CN107915499B CN201711246222.1A CN201711246222A CN107915499B CN 107915499 B CN107915499 B CN 107915499B CN 201711246222 A CN201711246222 A CN 201711246222A CN 107915499 B CN107915499 B CN 107915499B
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- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
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- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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Abstract
The repairing method of C/SiC ceramic-base composite material includes polishing the surface of sample, washing, drying, etching the sample with HF, washing, stoving, ultrasonic washing, stoving and soaking in Ni (NO)3)2·6H2And O in acetone solution, drying in vacuum, and wrapping the sample by graphite paper to expose the fracture. Putting the sample into a vacuum furnace, and introducing C2H2、H2And Ar, preserving heat for 10-150 h, and closing C2H2And H2Keeping the temperature for 10-100 min, and introducing C3H6Keeping the temperature for 5-12 h, and closing the C3H6Trichloromethylsilane and H are introduced2Keeping the temperature for 50-300H, taking out the sample, removing graphite paper, polishing and repairing the surface, putting the treated sample into a vacuum furnace, introducing trichloromethylsilane and H2And Ar, preserving the heat for 5-30 h, and spraying a composite coating consisting of yttrium silicate and mullite on the surface by adopting a plasma spraying method. The method can repair main damage easily generated in the service process of the C/SiC composite material, the composition of the material is not changed after the repair is finished, and the oxidation resistance of the material in a high-temperature environment is improved.
Description
Technical Field
The invention relates to a method for repairing a ceramic matrix composite, in particular to a method for repairing a C/SiC ceramic matrix composite.
Background
With the rapid development of the aerospace industry, light-weight, high-temperature-resistant and oxidation-resistant materials are more and more important for aerospace vehicles. The C/SiC composite material has the characteristics of low specific gravity, high temperature resistance, excellent chemical stability, energy absorption in multiple failure modes in the damage process, insensitivity to cracks and avoidance of large-area damage of the material. When the composite material is used as a turbine engine, a thermal protection device of an aerospace craft, a heat engine component and other parts, the weight of the aerospace craft can be effectively reduced, and the thrust-weight ratio of the aero-engine is improved.
The main application field of the C/SiC is often related to a high-temperature environment, the high-temperature environment can influence the occurrence and evolution of subsequent oxidation damage, besides thermal mismatch cracks generated in the preparation process, the C/SiC can also generate thermal damage cracks due to the mismatch of thermal expansion coefficients in the high-temperature oxidation service process, and the cracks can cause the reduction of the high-temperature oxidation resistance of the ceramic matrix composite material, so that the component is subjected to early failure damage or even catastrophic damage in the repeated use process. Therefore, the repair technology for the cracks generated in the preparation and high-temperature service processes of the C/SiC composite material becomes particularly important.
Chinese patent application No. 201410629485.0 discloses a method for repairing thermal damage cracks of ceramic matrix composite. The method directly and thoroughly grinds the whole SiC coating on the surface of the sample with the thermal damage cracks, and then the SiC coating is deposited again. The deposition surface can be smooth, the C/SiC composite material with the whole SiC coating ground can be opened and closed with air holes, so that the subsequent deposition of the matrix and the coating becomes more compact, and the density gradient is reduced; cracks formed inside the SiC matrix can be effectively repaired.
The Chinese patent with the application number of 201710307256.0 discloses a method for repairing defects of a carbon fiber reinforced silicon carbide composite material. The method can repair C f The main damage of the/SiC composite material, which is easily generated in the service process, comprises high-temperature airflow or particle ablation, mechanical damage and the like, can realize C f The defects of the SiC composite material are repaired, the raw materials are easy to obtain, the process is simple and convenient to control, and the use cost of the composite material is expected to be greatly reduced; after the repair is complete, the material composition is still C f The composition of the/SiC composite material is not changed.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art, and the invention aims to provide a C/SiC ceramic matrix composite repairing method which is characterized by comprising the following steps in sequence:
(1) polishing the surface of the sample, cleaning and drying;
(2) cleaning a fracture of a C/SiC ceramic matrix composite sample, corroding the fracture for 30-60 min by using HF with the mass fraction of 10-15%, and then cleaning and drying;
(3) placing the corroded sample in deionized water for ultrasonic cleaning for 20-40 min, and drying;
(4) soaking the dried sample in Ni (NO)3)2·6H2In acetone solution of O, Ni (NO)3)2∙6H2O
The mass fraction of the mixture is 0.6-3%, the time is 2-4 h, and the mixture is dried in vacuum;
(5) wrapping the dried sample in step (4) with graphite paper until the fracture is exposed, placing the sample in a vacuum furnace, and introducing C2H2、 H2And Ar, C2H2、H2And Ar ratio is 1: 1-25: 1-25 deg.C at 700-900 deg.C for 10-100 h, and thenClose C2H2And H2Heating to 900-1600 ℃, and preserving the heat for 10-100 min;
(6) introduction of C3H6，C3H6The ratio of Ar to Ar is 1: 2-5, the temperature is 800-1200 ℃, and the time is 5-50 h;
(7) close C3H6Trichloromethylsilane and H are introduced2， H2And CH3SiCl3The proportion is 1:
5-15 ℃, the temperature is 950-1250 ℃, the system pressure is 10-1000 Pa, and the time is 50-300 h;
(8) taking out the sample, removing the graphite paper, and grinding the repaired surface with a diamond grinding tool to make the repaired surface contact with the surface
The sample surfaces are parallel and have consistent roughness;
(9) putting the sample treated in the step (7) into a vacuum furnace, and introducing trichloromethylsilane and H2And Ar, H2And CH3SiCl3The proportion is 1: 5-15 ℃, 950-1250 ℃, 10-1000 Pa of pressure and 5-30 h of time.
(10) The yttrium silicate and mullite composite coating is sprayed on the surface of the sample by adopting a plasma spraying method, the chemical purity of the mullite powder is 99.5%, the powder granularity is 100-200 meshes, the chemical purity of the yttrium silicate powder is 99.448%, and the powder granularity is 100-200 meshes.
The invention has the technical effects that:
the invention provides a method for repairing a C/SiC ceramic matrix composite, which can repair main damages, including high-temperature airflow or particle ablation, mechanical damage and the like, which are easily generated in the service process of the C/SiC ceramic matrix composite, and can realize the repair of defects of the C/SiC ceramic matrix composite; after the repair is finished, the composition of the material is still C/SiC composite material, and the composition is not changed; the surface is coated to improve the oxidation resistance of the material in high temperature environment.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will occur to those skilled in the art upon reading the present specification and which fall within the limits of the appended claims.
Example 1
(1) Polishing the surface of the sample, cleaning and drying;
(2) cleaning a fracture of the C/SiC ceramic matrix composite sample, corroding the fracture for 40min by using HF with the mass fraction of 11%, and then cleaning and drying;
(3) placing the corroded sample in deionized water for ultrasonic cleaning for 30min, and drying;
(4) soaking the dried sample in Ni (NO)3)2·6H2In acetone solution of O, Ni (NO)3)2∙6H2O
The mass fraction of the mixture is 1.2 percent, the time is 4 hours, and vacuum drying is carried out;
(5) wrapping the dried sample in step (4) with graphite paper, placing in a vacuum furnace, and introducing C2H2、 H2And Ar, C2H2、H2And Ar ratio is 1: 15: 15 at 700 ℃ for 20h, and then C is switched off2H2And H2Heating to 1300 deg.C, and maintaining the temperature for 30 min;
(6) introduction of C3H6，C3H6The ratio of Ar to Ar is 1:3, the temperature is 900 ℃, and the time is 15 h;
(7) close C3H6Trichloromethylsilane and H are introduced2， H2And CH3SiCl3The proportion is 1:
8, the temperature is 950 ℃, the system pressure is 500Pa, and the time is 250 h;
(8) taking out the sample, removing the graphite paper, and grinding the repaired surface with a diamond grinding tool to make the repaired surface contact with the surface
The sample surfaces are parallel and have consistent roughness;
(9) putting the sample treated in the step (7) into a vacuum furnace, and introducing trichloromethylsilane and H2And Ar, H2And CH3SiCl3The proportion is 1: 10 at 1100 deg.C and pressure500Pa and 25 h.
(10) The yttrium silicate and mullite composite coating is sprayed on the surface of the sample by adopting a plasma spraying method, the chemical purity of mullite powder is 99.5 percent, the powder granularity is 100 meshes, the chemical purity of yttrium silicate powder is 99.448 percent, and the powder granularity is 100 meshes.
Example 2
(1) Polishing the surface of the sample, cleaning and drying;
(2) cleaning a fracture of the C/SiC ceramic matrix composite sample, corroding the fracture for 30min by using HF with the mass fraction of 13%, and then cleaning and drying;
(3) placing the corroded sample in deionized water for ultrasonic cleaning for 25min, and drying;
(4) soaking the dried sample in Ni (NO)3)2·6H2In acetone solution of O, Ni (NO)3)2∙6H2O
The mass fraction of the mixture is 1.5 percent, the time is 3 hours, and vacuum drying is carried out;
(5) wrapping the dried sample in step (4) with graphite paper, placing in a vacuum furnace, and introducing C2H2、 H2And Ar, C2H2、H2And Ar ratio is 1: 20: 20 at 900 ℃ for 15h, and then C is switched off2H2And H2Heating to 1500 deg.C, and maintaining the temperature for 20 min;
(6) introduction of C3H6，C3H6The ratio of Ar to Ar is 1:4, the temperature is 1200 ℃, and the time is 8 h;
(7) close C3H6Trichloromethylsilane and H are introduced2， H2And CH3SiCl3The proportion is 1:
12, the temperature is 1250 ℃, the system pressure is 800Pa, and the time is 200 h;
(8) taking out the sample, removing the graphite paper, and grinding the repaired surface with a diamond grinding tool to make the repaired surface contact with the surface
The sample surfaces are parallel and have consistent roughness;
(9) after the treatment of (7)The sample is put into a vacuum furnace, and trichloromethylsilane and H are introduced2And Ar, H2And CH3SiCl3The proportion is 1: 12, the temperature is 1100 ℃, the pressure is 750Pa, and the time is 15 h.
(10) The yttrium silicate and mullite composite coating is sprayed on the surface of the sample by adopting a plasma spraying method, the chemical purity of mullite powder is 99.5%, the powder granularity is 1200 meshes, the chemical purity of yttrium silicate powder is 99.448%, and the powder granularity is 200 meshes.
Claims (1)
1. The method for repairing the C/SiC ceramic matrix composite is characterized by comprising the following steps in sequence:
(1) polishing the surface of the sample, cleaning and drying;
(2) cleaning a fracture of a C/SiC ceramic matrix composite sample, and corroding for 30-60 min by using HF with the mass fraction of 10-15%;
(3) placing the corroded sample in deionized water for ultrasonic cleaning for 20-40 min, and drying;
(4) soaking the dried sample in Ni (NO)3)2·6H2In acetone solution of O, Ni (NO)3)2∙6H2O
The mass fraction of the mixture is 0.6-3%, the time is 2-4 h, and the mixture is dried in vacuum;
(5) wrapping the dried sample in step (4) with graphite paper until the fracture is exposed, placing the sample in a vacuum furnace, and introducing C2H2、 H2And Ar, C2H2、H2And Ar ratio is 1: 1-25: 1-25 ℃, the temperature is 700-900 ℃, the time is 10-100 h, and then C is closed2H2And H2Heating to 900-1600 ℃, and preserving the heat for 10-100 min;
(6) introduction of C3H6，C3H6The ratio of Ar to Ar is 1: 2-5, the temperature is 800-1200 ℃, and the time is 5-50 h;
(7) close C3H6Trichloromethylsilane and H are introduced2， H2And CH3SiCl3The proportion is 1:
5-15 ℃, the temperature is 950-1250 ℃, the system pressure is 10-1000 Pa, and the time is 50-300 h;
(8) taking out the sample, removing the graphite paper, and grinding the repaired surface with a diamond grinding tool to make the repaired surface contact with the surface
The sample surfaces are parallel and have consistent roughness;
(9) putting the sample treated in the step (8) into a vacuum furnace, and introducing trichloromethylsilane and H2And Ar, H2And CH3SiCl3The proportion is 1: 5-15 ℃, the temperature is 950-1250 ℃, the pressure is 10-1000 Pa, and the time is 5-30 h;
(10) the yttrium silicate and mullite composite coating is sprayed on the surface of the sample by adopting a plasma spraying method, the chemical purity of the mullite powder is 99.5%, the powder granularity is 100-200 meshes, the chemical purity of the yttrium silicate powder is 99.448%, and the powder granularity is 100-200 meshes.
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| CN101698975A (en) * | 2009-09-23 | 2010-04-28 | 北京航空航天大学 | Method for modifying carbonized pre-oxidized fiber preform interface by carbon nanotube |
| CN102584350A (en) * | 2012-02-09 | 2012-07-18 | 中南大学 | Preparation method for SiC/TaC ceramic complex-phase interface modified C/C composite material |
| CN104150958A (en) * | 2014-08-08 | 2014-11-19 | 苏州宏久航空防热材料科技有限公司 | Repair method for ceramic matrix composite material |
| CN104446666A (en) * | 2014-11-11 | 2015-03-25 | 西北工业大学 | Method for repairing heat damage crackles of ceramic based composite material |
| CN105384467A (en) * | 2015-12-14 | 2016-03-09 | 中国航空工业集团公司北京航空制造工程研究所 | Environmental barrier coating used for ceramic base composite material matrix, and making method thereof |
| CN106986664A (en) * | 2017-05-04 | 2017-07-28 | 中国人民解放军国防科学技术大学 | The restorative procedure of carbon fibre reinforced silicon carbide composite material defect |
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- 2017-12-01 CN CN201711246222.1A patent/CN107915499B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698975A (en) * | 2009-09-23 | 2010-04-28 | 北京航空航天大学 | Method for modifying carbonized pre-oxidized fiber preform interface by carbon nanotube |
| CN102584350A (en) * | 2012-02-09 | 2012-07-18 | 中南大学 | Preparation method for SiC/TaC ceramic complex-phase interface modified C/C composite material |
| CN104150958A (en) * | 2014-08-08 | 2014-11-19 | 苏州宏久航空防热材料科技有限公司 | Repair method for ceramic matrix composite material |
| CN104446666A (en) * | 2014-11-11 | 2015-03-25 | 西北工业大学 | Method for repairing heat damage crackles of ceramic based composite material |
| CN105384467A (en) * | 2015-12-14 | 2016-03-09 | 中国航空工业集团公司北京航空制造工程研究所 | Environmental barrier coating used for ceramic base composite material matrix, and making method thereof |
| CN106986664A (en) * | 2017-05-04 | 2017-07-28 | 中国人民解放军国防科学技术大学 | The restorative procedure of carbon fibre reinforced silicon carbide composite material defect |
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