CN115784760B - C/C composite material antioxidation coating and preparation method thereof - Google Patents
C/C composite material antioxidation coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of composite materials, and particularly discloses a C/C composite material antioxidation coating and a preparation method thereof, wherein the preparation method comprises the following steps: 1) Test C/CEmbedding the sample in the powder twice, taking out the sample after embedding twice each time under the protection of Ar atmosphere at high temperature, polishing, washing and drying to obtain a C/C-SiC sample; 2) SiB is taken 6 And Al 2 O 3 Mixing and ball milling the powder, and sieving to obtain mixed powder; 3) Adding silica sol and water into the mixed powder to prepare suspension; stirring after dispersing to obtain slurry suspension; 4) Heating a C/C-SiC sample, then placing the C/C-SiC sample into slurry suspension for hot dipping, cooling, taking out, placing the C/C-SiC sample into absolute ethyl alcohol for ultrasonic cleaning, taking out the C/C-SiC sample, and then heating; repeating the steps of soaking and ultrasonic treatment, and drying to obtain C/C-SiC-SiB 6 /Al 2 O 3 And (3) forming a C/C composite material antioxidation coating on the surface of the sample. The C/C composite material antioxidation coating prepared by the preparation method has self-repairing capability, and can be used for protecting the C/C composite material at high temperature and self-repairing the coating.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to an anti-oxidation coating of a C/C composite material and a preparation method thereof.
Background
The C/C composite material is widely applied to the fields of aerospace and the like (Shechan J E, bucsking K W, sullivan B J Carbon Carbon Composites [ J ] Annual Reviewof Materials Sciencc, 1994, 24:19-44 ]) because of the excellent high-temperature performance, but the C/C composite material is oxidized in an aerobic environment exceeding 723K, and the mechanical property is greatly reduced, so that the wide application of the C/C composite material in high-temperature oxidizing atmosphere is limited [ Yang Xin, huang Qizhong, su Zhean and the like ] the high-temperature oxidation resistance protection research of the C/C composite material is progressed [ J ]. Aerospace material technology, 2014 (1): 1-15 ].
Therefore, protecting the C/C composite from oxidation at high temperatures is a solutionKey. At present, the oxidation resistance methods of the C/C composite materials mainly comprise two methods: one is the matrix modification technology [ Yang Xing, cui Gong, ] associated with the current state of research [ J ] of matrix modification of C/C composite materials]Material guides, 2007, 21 (8): 22-24.]Another is the antioxidation coating technique [ Wu Heng, li Hejun, maChao, et al MoSi ] 2 -based oxidation protectivecoatings for SiC-coated carbon/carbon composites prepared by supersonicplasma spraying [J]. Journal of the European Ceramic Society， 2010， 30(15): 3267-3270.]. At present, the oxidation resistance coating is the most direct and effective method for improving the oxidation resistance of the C/C composite material.
Aiming at the research on the composite material antioxidant coating at home and abroad at present, the composite coating and the gradient coating are easy to find that the composite coating and the gradient coating have great development space and potential [ Yang Xing, cui Gong, ] the research progress of the C/C composite material antioxidant coating [ J ]]Carbon (4) 16-21, 11.]. The literature indicates that SiB 6 Oxidation reaction can occur at 800 ℃ or above, and the oxidation product is SiO 2 And B 2 O 3 [MATSUSHITA J，KOMARNENI S.High temperature oxidation of siliconhexaboride ceramics[J]．Materials Research Bulletin，2001，36(5):1083-1089.]. Under the action of high temperature, the two oxidation products can form borosilicate glass with certain fluidity and good sealing property, which is beneficial to self-repairing of C/C composite material cracks at high temperature. But of single-component SiB 6 The coating does not provide protection for the C/C matrix for a long period of time, and thus there is a need for an oxidation-resistant coating for protection and self-repair of C/C composites at high temperatures and a method for preparing the same.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a C/C composite material antioxidation coating with certain self-repairing capability and used for protecting and coating self-repairing at high temperature of the C/C composite material and a preparation method thereof.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
a preparation method of a C/C composite material antioxidation coating comprises the following steps:
1) The SiC inner coating is prepared by a two-step embedding method: burying the C/C sample in powder twice, preserving heat for 2-8 hours under the protection of Ar atmosphere at the high temperature of 2000-2400 ℃ each time, taking out the sample after twice embedding, polishing, washing and drying to obtain the C/C-SiC sample; wherein, the primary embedded powder is obtained by mixing silicon powder, carbon powder and alumina powder, and the secondary embedded powder is obtained by mixing silicon powder, carbon powder and boron oxide powder;
2) SiB is taken 6 And Al 2 O 3 Mixing and ball milling the powder, and sieving to obtain mixed powder, wherein Al 2 O 3 The mass fraction of the powder is 5-40wt%;
3) According to the volume ratio of 1: (2-6) taking silica sol and water; then adding the mixed powder obtained in the step 2) to prepare a suspension with the concentration of 0.1-0.3 g/mL; after the suspension is subjected to ultrasonic dispersion, stirring for 12-24 hours to obtain slurry suspension;
4) Heating a C/C-SiC sample at 150-300 ℃ for 5-20 min, taking out, directly putting the C/C-SiC sample into slurry suspension for thermal impregnation, taking out the C/C-SiC sample after the C/C-SiC sample is cooled in slurry, putting the C/C-SiC sample into absolute ethyl alcohol for ultrasonic cleaning for 2-5 min, taking out the C/C-SiC sample and heating the C/C-SiC sample after the C/C-SiC sample is cleaned; repeating the above soaking and ultrasonic cleaning processes, and drying the cleaned sample to obtain C/C-SiC-SiB 6 /Al 2 O 3 Sample, C/C-SiC-SiB 6 /Al 2 O 3 And C/C composite material antioxidation coating is formed on the surface of the sample.
Further, in the powder material once embedded in the step 1), the mass percentages of the silicon powder, the carbon powder and the alumina powder are respectively 60-80%, 15-20% and 5-20%.
Further, in the secondarily embedded powder in the step 1), the mass percentages of the silicon powder, the carbon powder and the boron oxide powder are respectively 60-80%, 15-20% and 5-20%.
Further, the ball milling time in the step 2) is 6-12 hours.
Further, the screen in the step 2) is a 180-mesh screen.
Further, in the step 3), the ultrasonic dispersion time is 20-60 min.
Further, the drying time in the step 4) is 60-180 min.
The C/C composite material antioxidation coating is prepared by adopting the preparation method of the C/C composite material antioxidation coating.
Compared with the prior art, the invention has the following technical effects:
1. SiB prepared by the invention 6 /Al 2 O 3 Oxidation-resistant coating, which can form flowable SiO at high temperatures 2 ·B 2 O 3 Can be used for high-temperature protection and crack self-repairing of C/C composite materials, al 2 O 3 Can also be combined with SiO 2 Mullite is generated at high temperature, the melting point of the coating is improved, a more compact and firm glass protection layer is formed, the coating is toughened, and the C/C-SiC-SiB 6 /Al 2 O 3 After 230h of oxidation in 1573K air, the weight loss is only 0.57%.
2. The C/C composite material antioxidation coating is prepared by the hot dipping method, the coating prepared by the method has strong binding force, the structure and the composition of the coating can be controlled manually to a certain extent, and the problems of coating falling and cracking caused by thermal stress in the thermal cycle process of the traditional preparation process are avoided.
3. The method has the advantages of mild reaction conditions, easy realization, simple preparation process, simple requirements on experimental equipment, low cost, easy control of the process and environmental friendliness.
4. The thickness of the coating can be well regulated and controlled by controlling the concentration of silica sol, the concentration of slurry, the dipping times and the like.
Drawings
FIG. 1 is a XRD contrast pattern of example 3 of the present invention, before and after oxidation of C/C-SiC-SiB6/Al2O 3;
FIG. 2 is a C/C-SiC-SiB in example 3 of the present invention 6 /Al 2 O 3 A comparison of the scans of the front and rear surfaces before and after oxidation;
FIG. 3 is a C/C-SiC-SiB in example 3 of the present invention 6 /Al 2 O 3 Isothermal antioxidant profile of the sample in 1573K air.
Detailed Description
The following examples illustrate the invention in further detail.
Examples
Example 1
A preparation method of a C/C composite material antioxidation coating comprises the following steps:
1) The SiC inner coating is prepared by a two-step embedding method: placing 75% of silicon powder, 17.5% of carbon powder and 7.5% of alumina powder in a ball milling tank according to the mass fraction ratio, ball milling and mixing for 6 hours, placing the mixture into a graphite crucible, burying the polished, cleaned and dried C/C composite material into the mixed powder, placing the graphite crucible into a vacuum reaction furnace, and preserving heat for 2 hours at 2000 ℃ under the protection of Ar atmosphere. And naturally cooling to room temperature after heat preservation is finished, taking out the C/C composite material after primary embedding, polishing particles adhered to the surface by using sand paper, washing and drying.
Placing silicon powder, carbon powder and boron oxide powder in a ball milling tank according to the mass fraction ratio of 75%, 17.5% and 7.5% for ball milling and mixing for 6 hours, placing the mixture into a graphite crucible, embedding the primary-embedded and processed C/C composite material into the mixed powder, placing the graphite crucible into a vacuum reaction furnace, preserving the temperature at 2200 ℃ for 2 hours under Ar atmosphere protection, naturally cooling to room temperature after the heat preservation is finished, taking out the secondary-embedded C/C composite material, polishing particles adhered on the surface by sand paper, washing and drying to obtain the C/C-SiC sample.
2) Weigh 3.8g SiB 6 Powder and 0.2g of Al 2 O 3 Mixing the powder and the powder, ball milling for 6 hours, and sieving with a 180-mesh sieve.
3) Measuring 10mL of silica sol by using a measuring cylinder, placing the silica sol in a beaker, adding 30mL of water, weighing 4g of mixed powder, and preparing 0.1g/mL of suspension; and (3) after the suspension is subjected to ultrasonic dispersion for 30min, magnetically stirring for 12h to obtain a uniformly dispersed slurry suspension.
4) Heating a C/C-SiC sample in a muffle furnace at 200 ℃ for 10min, taking out the sample, directly placing the sample into a beaker filled with slurry for heat impregnation, taking out the sample after the sample is cooled in the slurry, placing the sample into the beaker filled with absolute ethyl alcohol for ultrasonic cleaning for 3min, taking out the sample after cleaning, and placing the sample into the muffle furnace for heat impregnationAnd (5) heating. The above-described dipping and ultrasonic cleaning processes are repeated. By observation and weighing, the thickness of the coating can be estimated. After the weight of the sample is increased by 0.0552g, the cleaned sample is placed in a baking oven at 60 ℃ for drying for 120min, and the C/C-SiC-SiB can be obtained after drying 6 /Al 2 O 3 Sample, C/C-SiC-SiB 6 /Al 2 O 3 And C/C composite material antioxidation coating is formed on the surface of the sample.
Example 2
A preparation method of a C/C composite material antioxidation coating comprises the following steps:
1) The SiC undercoating was prepared by a two-step embedding process, this step being the same as that in example 1.
2) Weigh 3.6g SiB 6 Powder and 0.4g of Al 2 O 3 Mixing the powder and the powder, ball milling for 6 hours, and sieving with a 180-mesh sieve.
3) Measuring 10mL of silica sol by using a measuring cylinder, placing the silica sol in a beaker, adding 30mL of water, weighing 4g of mixed powder, and preparing 0.1g/mL of suspension; after the suspension is dispersed for 30min by ultrasonic, the slurry suspension which is uniformly dispersed is obtained by magnetic stirring for 12h.
4) Heating a C/C-SiC sample in a muffle furnace at 200 ℃ for 10min, taking out the sample, directly putting the sample into a beaker filled with slurry for heat impregnation, taking out the sample after the sample is cooled in the slurry, putting the sample into the beaker filled with absolute ethyl alcohol for ultrasonic cleaning for 3min, taking out the sample after cleaning, and putting the sample into the muffle furnace for heating. The above-described dipping and ultrasonic cleaning processes are repeated. By observation and weighing, the thickness of the coating can be estimated. After the weight of the sample is increased by 0.0493g, the cleaned sample is placed in a baking oven at 60 ℃ for drying for 120min, and the C/C-SiC-SiB can be obtained after drying 6 /Al 2 O 3 Sample, C/C-SiC-SiB 6 /Al 2 O 3 And C/C composite material antioxidation coating is formed on the surface of the sample.
Example 3
A preparation method of a C/C composite material antioxidation coating comprises the following steps:
1) The SiC undercoating was prepared by a two-step embedding process, this step being the same as that in example 1.
2) Weigh 3.2g SiB 6 Powder and 0.8g of Al 2 O 3 Mixing the powder and the powder, ball milling for 6 hours, and sieving with a 180-mesh sieve.
3) Measuring 10mL of silica sol by using a measuring cylinder, placing the silica sol in a beaker, adding 30mL of water, weighing 4g of mixed powder, and preparing 0.1g/mL of suspension; after the suspension is dispersed for 30min by ultrasonic, the slurry suspension which is uniformly dispersed is obtained by magnetic stirring for 12h.
4) Heating a C/C-SiC sample in a muffle furnace at 200 ℃ for 10min, taking out the sample, directly putting the sample into a beaker filled with slurry for heat impregnation, taking out the sample after the sample is cooled in the slurry, putting the sample into the beaker filled with absolute ethyl alcohol for ultrasonic cleaning for 3min, taking out the sample after cleaning, and putting the sample into the muffle furnace for heating. The above-described dipping and ultrasonic cleaning processes are repeated. By observation and weighing, the thickness of the coating can be estimated. After the weight of the sample is increased by 0.0523g, the cleaned sample is placed in a baking oven at 60 ℃ for drying for 120min, and the C/C-SiC-SiB can be obtained after drying 6 /Al 2 O 3 Sample, C/C-SiC-SiB 6 /Al 2 O 3 And C/C composite material antioxidation coating is formed on the surface of the sample.
Example 4
The preparation method of the C/C composite material antioxidant coating is carried out according to the method in the embodiment 1, and the difference is that:
the powder embedded once in the step 1) is obtained by mixing 60%, 20% and 20% of silicon powder, carbon powder and alumina powder according to the mass fraction ratio; the secondary embedded powder is obtained by mixing 60%, 20% and 20% of silicon powder, carbon powder and boron oxide powder according to the mass fraction ratio;
2.4g SiB weighed in step 2) 6 Powder and 1.6g of Al 2 O 3 Powder, wherein the ball milling time is 10 hours;
in the step 3), 10mL of silica sol and 20mL of water are taken, 6g of mixed powder is weighed, and 0.2g/mL of suspension is prepared; and the ultrasonic dispersion time is 20min;
heating the C/C-SiC sample in the step 4) in a muffle furnace at 150 ℃ for 20min, ultrasonically cleaning the C/C-SiC sample by using absolute ethyl alcohol for 3min, weighing the C/C-SiC sample by 0.0571g, and drying the cleaned C/C-SiC sample in an oven at 60 ℃ for 60min.
Example 5
The preparation method of the C/C composite material antioxidant coating is carried out according to the method in the embodiment 1, and the difference is that:
the powder embedded once in the step 1) is obtained by mixing silicon powder, carbon powder and alumina powder according to the mass fraction ratio of 80%, 15% and 5%; the secondary embedded powder is obtained by mixing silicon powder, carbon powder and boron oxide powder according to the mass fraction ratio of 80%, 15% and 5%;
the ball milling time in the step 2) is 12 hours;
in the step 3), 10mL of silica sol and 60mL of water are taken, 21g of mixed powder is weighed, and 0.3g/mL of suspension is prepared; and the ultrasonic dispersion time is 60min;
heating the C/C-SiC sample in the step 4) in a muffle furnace at 300 ℃ for 5min, ultrasonically cleaning the C/C-SiC sample by using absolute ethyl alcohol for 5min, adding 0.0600g of weight of the sample, and drying the cleaned sample in an oven at 60 ℃ for 180min.
Performance detection
The C/C-SiC-SiB obtained in each of the above-mentioned embodiments 6 /Al 2 O 3 The test sample was placed in a silicon carbide rod high temperature furnace and subjected to an antioxidant test in an air atmosphere of 1573K.
FIG. 1 (a) is a C/C-SiC-SiB prepared in example 3 of the method of the present invention 6 /Al 2 O 3 XRD patterns before oxidation, no SiC undercoating was detected, and SiB was prepared by this method 6 /Al 2 O 3 The coating is uniform and compact, the thickness is proper, and a small amount of SiO 2 From silica sol. FIG. 1 (b) is a C/C-SiC-SiB prepared in example 2 of the method of the present invention 6 /Al 2 O 3 XRD patterns after oxidation, it can be seen that C/C-SiC-SiB 6 /Al 2 O 3 After oxidation B is produced 2 O 3 ·SiO 2 、Al 2 O 3 ·SiO 2 Consistent with the expectations;
FIG. 2 (a) is a C/C-SiC-SiB in example 3 of the method of the present invention 6 /Al 2 O 3 According to the scanning image of the surface before oxidation, siB6 and Al2O3 mixed powder is firstly agglomerated in silica sol and then uniformly distributed on the surface of a sample, and although certain cracks exist on the surface, the cracks only exist between the silica sol and are not penetrable; FIG. 2 (b) is a C/C-SiC-SiB in example 3 of the method of the present invention 6 /Al 2 O 3 The surface scanning image after oxidation shows that the crack disappears, the crack is non-penetrating before oxidation, the surface of the coating is compact and smooth, the generated air holes are healed by the glass phase, and the coating has certain self-healing capability;
FIG. 3 is a C/C-SiC-SiB prepared in example 3 of the method of the present invention 6 /Al 2 O 3 Isothermal antioxidant profile of the sample in 1573K air, before 25h due to SiB 6 The oxidation product is generated, the sample is in the weight increasing stage, and the weight loss rate after 230 hours of oxidation is only 0.57%.
Claims (8)
1. A preparation method of a C/C composite material antioxidation coating is characterized by comprising the following steps: the method comprises the following steps:
1) The SiC inner coating is prepared by a two-step embedding method: burying the C/C sample in powder twice, preserving heat for 2-8 hours under the protection of Ar atmosphere at the high temperature of 2000-2400 ℃ each time, taking out the sample after twice embedding, polishing, washing and drying to obtain the C/C-SiC sample; wherein, the primary embedded powder is obtained by mixing silicon powder, carbon powder and alumina powder, and the secondary embedded powder is obtained by mixing silicon powder, carbon powder and boron oxide powder;
2) SiB is taken 6 And Al 2 O 3 Mixing and ball milling the powder, and sieving to obtain mixed powder, wherein Al 2 O 3 The mass fraction of the powder is 5-40wt%;
3) According to the volume ratio of 1: (2-6) taking silica sol and water; then adding the mixed powder obtained in the step 2) to prepare a suspension with the concentration of 0.1-0.3 g/mL; after the suspension is subjected to ultrasonic dispersion, stirring for 12-24 hours to obtain slurry suspension;
4) Heating the C/C-SiC sample at 150-300 ℃ for 5-20 min, taking out, directly putting into slurry suspension for thermal impregnation, taking out after the sample is cooled in slurry, and then putting into absolute ethyl alcohol for superCleaning with sound for 2-5 min, taking out the sample after cleaning, and heating; repeating the above soaking and ultrasonic cleaning processes, and drying the cleaned sample to obtain C/C-SiC-SiB 6 /Al 2 O 3 Sample, C/C-SiC-SiB 6 /Al 2 O 3 And C/C composite material antioxidation coating is formed on the surface of the sample.
2. The method for preparing the C/C composite material antioxidant coating according to claim 1, wherein the mass percentages of the silicon powder, the carbon powder and the alumina powder in the powder embedded in the step 1) are respectively 60-80%, 15-20% and 5-20%.
3. The method for preparing the C/C composite material antioxidant coating according to claim 1, wherein the mass percentages of the silicon powder, the carbon powder and the boron oxide powder in the secondarily embedded powder in the step 1) are respectively 60-80%, 15-20% and 5-20%.
4. The method for preparing the C/C composite material antioxidant coating according to claim 1, wherein the ball milling time in the step 2) is 6-12 hours.
5. The method for preparing an oxidation resistant coating according to claim 1, wherein the screen in the step 2) is a 180 mesh screen.
6. The method for preparing the C/C composite material antioxidant coating according to claim 1, wherein the ultrasonic dispersion time in the step 3) is 20-60 min.
7. The method for preparing the C/C composite material antioxidant coating according to claim 1, wherein the drying time in the step 4) is 60-180 min.
8. A C/C composite oxidation resistant coating, characterized in that it is produced by a process for producing a C/C composite oxidation resistant coating according to any one of claims 1 to 7.
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