CN113563119A - Preparation method of C/C composite material surface oxidation-resistant coating - Google Patents
Preparation method of C/C composite material surface oxidation-resistant coating Download PDFInfo
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Abstract
The invention discloses a preparation method of a C/C composite material surface antioxidant coating, which comprises the following steps: embedding a SiC coating on the surface of the C/C composite material by adopting an embedding method to obtain the C/C composite material protected by the SiC coating; ZrSi is sprayed on the surface of the C/C composite material protected by the SiC coating2Obtaining ZrSi on the surface of the C/C composite material by using-SiC powder2-SiC/SiC oxidation resistant coating. The SiC in the outer coating is consistent with the SiC in the inner coating, so that the difference of the thermal expansion coefficients of the inner coating and the outer coating can be effectively reduced, and the generation of cracks caused by uneven thermal stress of the inner coating and the outer coating, even the peeling of the outer coating, can be relieved; the coating is a gradient coating system, the coefficient of thermal expansion is distributed in a gradient manner from the inner coating to the outer coating, the thermal stress of the coating is effectively relieved, and the oxidation resistance of the coating system is improved.
Description
Technical Field
The invention belongs to the technical field of protective materials, and relates to a preparation method of an antioxidant coating on the surface of a C/C composite material.
Background
The C/C composite material has excellent high-temperature thermodynamic performance, so that the C/C composite material is one of the most ideal high-temperature thermal structure protective materials. However, its application is limited by the problem of susceptibility to oxidation in high temperature aerobic environments, and the most effective method is currently to use external coating techniques. The embedding method and the supersonic plasma spraying (SAPS) method have been developed in recent yearsThe embedding method can obtain a coating with controllable phase and compact coating; the plasma arc temperature of the SAPS method is close to 10000 ℃, the SAPS method can be used for preparing ultrahigh and high-melting-point ceramic coatings, and the obtained coatings have strong interface bonding force and are compact. Current external coating technology mainly utilizes the ability of silicon carbide (SiC) ceramics to oxidize at high temperatures to produce limited, mobile, glassy phase SiO2The high temperature oxidation resistance of the C/C composite material is improved by healing the microcracks and pores of the coating, but the SiC reacts with oxygen to generate SiO at 1300 ℃ and above2So that below this temperature oxygen still readily enters the interior of the coating and reacts with the C/C matrix and simultaneously oxidizes the SiO formed2The fluidity is poor in the medium and low temperature region, and all defects such as cracks and pores in the coating cannot be healed, so that the oxidation resistance of the coating is finally failed. The oxidation resistance of the currently adopted oxidation resistant coating at 1500 ℃ is still not ideal.
Disclosure of Invention
The invention aims to provide a preparation method of a C/C composite material surface oxidation-resistant coating, which solves the problem that all the defects of cracks, pores and the like in the coating cannot be healed in the prior art.
The technical scheme adopted by the invention is that the preparation method of the C/C composite material surface antioxidant coating comprises the following steps:
step 1, embedding a SiC coating on the surface of the C/C composite material by adopting an embedding method to obtain the C/C composite material protected by the SiC coating;
step 2, spraying ZrSi on the surface of the C/C composite material protected by the SiC coating2Obtaining ZrSi on the surface of the C/C composite material by using-SiC powder2-SiC/SiC oxidation resistant coating.
The invention is also characterized in that:
and (3) polishing, cleaning and drying the C/C composite material in sequence before the step 1.
Step 1 the embedding process is as follows: embedding the C/C composite material into the embedded powder, taking Ar as protective gas, raising the temperature to 1900-2100 ℃ at the speed of 8-10 ℃/min, preserving the temperature for 1-2h, and naturally cooling to normal temperature to obtain the C/C composite material protected by the SiC coating.
The preparation process of the embedded powder comprises the following steps: 65 to 85 percent of Si powder, 8 to 16 percent of C powder and 7 to 19 percent of Al powder2O3And mixing the powder, placing the mixture in a resin ball milling tank, and mixing for 2-4h to obtain the embedded powder.
ZrSi2The preparation method of the-SiC powder comprises the following steps:
step A, 60 to 90 wt.% of ZrSi2Uniformly mixing 10-40 wt.% of SiC powder by adopting a planetary ball mill wet milling method to obtain mixed powder;
b, mixing and stirring 40-50 wt.% of mixed powder, 6-9 wt.% of binder and 44-51 wt.% of distilled water for 2 hours to obtain mixed slurry;
and C: granulating the mixed slurry by adopting a centrifugal sprayer to obtain spherical ZrSi2-SiC powder.
The inlet temperature of the centrifugal spraying machine is 280-320 ℃, and the outlet temperature is 110-140 ℃.
The specific process of the step 2 is as follows: ZrSi is sprayed by adopting a supersonic plasma spraying method2Spraying SiC powder on the surface of the C/C composite material protected by the SiC coating to obtain ZrSi on the surface of the C/C composite material2-SiC/SiC oxidation resistant coating.
The technological parameters of the supersonic plasma spraying method are as follows: the power is 30-50KW, the Ar flow is 65-80L/min, the powder feeding amount is 10-40g/min, and the spraying distance is 80-120 mm.
The invention has the beneficial effects that:
according to the preparation method of the C/C composite material surface antioxidant coating, the components of SiC in the outer coating are consistent with those of the inner coating, so that the difference of the thermal expansion coefficients of the inner coating and the outer coating can be effectively reduced, the generation of cracks caused by uneven thermal stress of the inner coating and the outer coating is relieved, and even the peeling of the outer coating is caused; the coating is a gradient coating system, the coefficient of thermal expansion is distributed in a gradient manner from an inner coating to an outer coating, the thermal stress of the coating is effectively relieved, and the oxidation resistance of the coating system is improved; ZrSi2And SiC is oxidized at high temperature to generate glass phase SiO2Not only can heal the defects of pores, cracks and the like in the coating, improve the density of the coating and prevent oxygen from entering and damaging the coatingLayer, and may be mixed with ZrSi2ZrO of (2)2React to generate SiC (alpha)SIC＝4.5×10-6) ZrSiO with approximate coefficient of thermal expansion4(αZrSiO4＝4.9×10-6)，ZrSiO4The inorganic composite material has excellent oxidation resistance, and can effectively relieve the thermal stress of the coating and reduce the generation and propagation of coating cracks when used as random phase nail piercing in the coating.
Drawings
FIG. 1 shows ZrSi prepared by the method for preparing the anti-oxidation coating on the surface of the C/C composite material2-surface secondary electron morphology of SiC/SiC composite coating;
FIG. 2 shows ZrSi prepared by the method for preparing the anti-oxidation coating on the surface of the C/C composite material2-SiC3The secondary electron appearance of the surface of the/SiC composite coating after being oxidized for 97h at 1500 ℃.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
A preparation method of a C/C composite material surface oxidation resistant coating comprises the following steps:
step 1, grinding and polishing the C/C composite material by using sand paper, ultrasonically cleaning the C/C composite material by using absolute ethyl alcohol for 20-40min, and then drying the C/C composite material in an oven at 70-100 ℃ for 0.5-1 h.
Step 2, embedding the SiC coating on the surface of the C/C composite material by adopting an embedding method to obtain the C/C composite material protected by the SiC coating;
specifically, 65-85% of Si powder, 8-16% of C powder and 7-19% of Al powder2O3And mixing the powder, placing the mixture in a resin ball milling tank, and mixing for 2-4h to obtain the embedded powder. Embedding the C/C composite material into embedded powder in a graphite crucible, placing the graphite crucible in a high-temperature graphitization heat treatment furnace, taking Ar as protective gas, heating to 1900-2100 ℃ at the speed of 8-10 ℃/min, preserving the heat for 1-2h, and naturally cooling to normal temperature to obtain the C/C composite material protected by the SiC coating.
Step 3, 60 to 90 wt.% of ZrSi210-40 wt.% of SiC powder is uniformly mixed by a planetary ball mill wet milling method to obtain mixed powderA body; mixing and stirring 40-50 wt.% of mixed powder, 6-9 wt.% of binder and 44-51 wt.% of distilled water for 2 hours to obtain mixed slurry; granulating the mixed slurry by adopting a centrifugal sprayer, wherein the inlet temperature of the centrifugal sprayer is 280-320 ℃, and the outlet temperature of the centrifugal sprayer is 110-140 ℃ to obtain the spherical ZrSi2-SiC powder; fixing the SiC coating protected C/C composite material by using a special clamp, and carrying out supersonic plasma spraying on ZrSi2Spraying SiC powder on the surface of the C/C composite material protected by the SiC coating to obtain ZrSi on the surface of the C/C composite material2-SiC/SiC oxidation resistant coatings; the technological parameters of the supersonic plasma spraying method are as follows: the power is 30-50KW, the Ar flow is 65-80L/min, the powder feeding amount is 10-40g/min, and the spraying distance is 80-120 mm.
ZrSi in the oxidation resistant coating2The oxidation reaction starts at 500 ℃ and when the temperature is increased to 900 ℃, ZrO can be generated2、SiO2And oxidation products such as Si, and a sufficient amount of SiO can be formed in the coating by adding 10-40 wt.% of SiC2Glassy phase, low viscosity SiO at high temperature2And Si can fully heal microcracks and pores in the coating, and the oxidation product ZrO2Phase and SiO2ZrSiO formed by reaction4Can inhibit SiO2And (3) volatilizing the glass phase, and keeping the weight of the coating sample to be increased after static oxidation at 1500 ℃ for 80-100 h.
Through the mode, the preparation method of the C/C composite material surface antioxidant coating has the advantages that the components of SiC in the outer coating are consistent with those of the inner coating, so that the difference of the thermal expansion coefficients of the inner coating and the outer coating can be effectively reduced, the generation of cracks caused by uneven thermal stress of the inner coating and the outer coating, and even the peeling of the outer coating is relieved; the coating is a gradient coating system, the coefficient of thermal expansion is distributed in a gradient manner from an inner coating to an outer coating, the thermal stress of the coating is effectively relieved, and the oxidation resistance of the coating system is improved; ZrSi2And SiC is oxidized at high temperature to generate glass phase SiO2Not only can heal the defects of pores, cracks and the like in the coating, improve the density of the coating, prevent oxygen from entering and damaging the coating, but also can be mixed with ZrSi2ZrO of (2)2React to generate SiC (alpha)SiC＝4.5×10-6) ZrSiO with approximate coefficient of thermal expansion4(αZrSiO4＝4.9×10-6)，ZrSiO4The inorganic composite material has excellent oxidation resistance, and can effectively relieve the thermal stress of the coating and reduce the generation and propagation of coating cracks when used as random phase nail piercing in the coating.
Example 1
Step 1, grinding and polishing the C/C composite material by using sand paper, ultrasonically cleaning the C/C composite material for 25min by using absolute ethyl alcohol, and then drying the C/C composite material for 1h in an oven at the temperature of 80 ℃;
and 2, mixing 70gSi powder, 15g C powder and 10g of SiC powder, putting the mixture into a resin ball milling tank, and mixing for 3 hours to obtain embedded powder. Embedding the C/C composite material into embedded powder in a graphite crucible, placing the graphite crucible in a high-temperature graphitization heat treatment furnace, taking Ar as protective gas, heating to 1900 ℃ at the speed of 8 ℃/min, preserving the temperature for 2h, and naturally cooling to normal temperature to obtain the C/C composite material protected by the SiC coating;
step 3, 80gZrSi is added220g of SiC powder is uniformly mixed by a planetary ball mill wet milling method to obtain mixed powder; mixing and stirring 45g of mixed powder, 6g of binder and 49g of distilled water for 2 hours to obtain mixed slurry; granulating the mixed slurry by a centrifugal sprayer at the inlet temperature of 290 ℃ and the outlet temperature of 120 ℃ to obtain spherical ZrSi2-SiC powder; fixing the SiC coating protected C/C composite material by using a special clamp, and carrying out supersonic plasma spraying on ZrSi2Spraying SiC powder on the surface of the C/C composite material protected by the SiC coating to obtain ZrSi on the surface of the C/C composite material2-SiC/SiC oxidation resistant coatings; the technological parameters of the supersonic plasma spraying method are as follows: the power is 30KW, the Ar flow is 75L/min, the powder feeding amount is 20g/min, and the spraying distance is 90 mm.
Example 2
Step 1, grinding and polishing the C/C composite material by using sand paper, ultrasonically cleaning the C/C composite material for 35min by using absolute ethyl alcohol, and then drying the C/C composite material for 1h in an oven at the temperature of 80 ℃;
and 2, mixing 75gSi powder, 12g C powder and 13g SiC powder, putting the mixture into a resin ball milling tank, and mixing for 3.5 hours to obtain embedded powder. Embedding the C/C composite material into embedded powder in a graphite crucible, placing the graphite crucible in a high-temperature graphitization heat treatment furnace, taking Ar as protective gas, raising the temperature to 2000 ℃ at the speed of 9 ℃/min, preserving the heat for 2h, and naturally cooling to normal temperature to obtain the C/C composite material protected by the SiC coating;
step 3, 70gZrSi230g of SiC powder is uniformly mixed by a planetary ball mill wet milling method to obtain mixed powder; mixing and stirring 44g of mixed powder, 5g of binder and 51g of distilled water for 2 hours to obtain mixed slurry; granulating the mixed slurry by a centrifugal sprayer at the inlet temperature of 300 ℃ and the outlet temperature of 125 ℃ to obtain spherical ZrSi2-SiC powder; fixing the SiC coating protected C/C composite material by using a special clamp, and carrying out supersonic plasma spraying on ZrSi2Spraying SiC powder on the surface of the C/C composite material protected by the SiC coating to obtain ZrSi on the surface of the C/C composite material2-SiC/SiC oxidation resistant coatings; the technological parameters of the supersonic plasma spraying method are as follows: the power is 40KW, the Ar flow is 70L/min, the powder feeding amount is 30g/min, and the spraying distance is 100 mm. ZrSi is obtained on the surface of the C/C composite material in the embodiment2The surface secondary electron morphology of the-SiC/SiC oxidation resistant coating is shown in figure 1, from which ZrSi can be seen2The SiC coating is compact and has no obvious pores and microcracks, which shows that the process parameters can prepare the coating meeting the use requirements. ZrSi obtained on the surface of the C/C composite material in this example2The surface secondary electron morphology of the-SiC/SiC oxidation resistant coating after being oxidized for 97h at 1500 ℃ is shown in figure 2, and it can be seen from the figure that the surface of the coating sample is still smooth and compact after being oxidized for 97h at 1500 ℃, and the coating sample benefits from the generated glass phase SiO2The micro cracks and pores in the coating are healed in time, oxygen is prevented from entering, and the oxidation resistance of the coating is further improved.
Example 3
Step 1, grinding and polishing the C/C composite material by using sand paper, ultrasonically cleaning the C/C composite material for 40min by using absolute ethyl alcohol, and then drying the C/C composite material for 1h in an oven at the temperature of 80 ℃;
and 2, mixing 80gSi powder, 12g C powder and 8g of SiC powder, putting the mixture into a resin ball milling tank, and mixing for 3 hours to obtain embedded powder. Embedding the C/C composite material into embedded powder in a graphite crucible, placing the graphite crucible in a high-temperature graphitization heat treatment furnace, taking Ar as protective gas, heating to 2100 ℃ at the speed of 10 ℃/min, preserving heat for 2h, and naturally cooling to normal temperature to obtain the C/C composite material protected by the SiC coating;
step 3, 60gZrSi240g of SiC powder is uniformly mixed by a planetary ball mill wet milling method to obtain mixed powder; mixing and stirring 50g of mixed powder, 6g of binder and 44g of distilled water for 2 hours to obtain mixed slurry; granulating the mixed slurry by a centrifugal sprayer at the inlet temperature of 320 ℃ and the outlet temperature of 135 ℃ to obtain spherical ZrSi2-SiC powder; fixing the SiC coating protected C/C composite material by using a special clamp, and carrying out supersonic plasma spraying on ZrSi2Spraying SiC powder on the surface of the C/C composite material protected by the SiC coating to obtain ZrSi on the surface of the C/C composite material2-SiC/SiC oxidation resistant coatings; the technological parameters of the supersonic plasma spraying method are as follows: the power is 50KW, the Ar flow is 75L/min, the powder feeding amount is 40g/min, and the spraying distance is 110 mm.
Claims (8)
1. A preparation method of an anti-oxidation coating on the surface of a C/C composite material is characterized by comprising the following steps:
step 1, embedding a SiC coating on the surface of the C/C composite material by adopting an embedding method to obtain the C/C composite material protected by the SiC coating;
step 2, spraying ZrSi on the surface of the C/C composite material protected by the SiC coating2Obtaining ZrSi on the surface of the C/C composite material by using-SiC powder2-SiC/SiC oxidation resistant coating.
2. The method for preparing the C/C composite material surface oxidation resistant coating according to claim 1, wherein the C/C composite material is sequentially polished, cleaned and dried before the step 1.
3. The preparation method of the C/C composite material surface oxidation resistant coating according to claim 1, characterized in that the embedding process in step 1 is as follows: embedding the C/C composite material into the embedded powder, taking Ar as protective gas, raising the temperature to 1900-2100 ℃ at the speed of 8-10 ℃/min, preserving the temperature for 1-2h, and naturally cooling to normal temperature to obtain the C/C composite material protected by the SiC coating.
4. The preparation method of the C/C composite material surface oxidation resistant coating according to claim 3, characterized in that the preparation process of the embedded powder material is as follows: 65 to 85 percent of Si powder, 8 to 16 percent of C powder and 7 to 19 percent of Al powder2O3And mixing the powder, placing the mixture in a resin ball milling tank, and mixing for 2-4h to obtain the embedded powder.
5. The method for preparing the C/C composite material surface oxidation resistant coating according to claim 1, wherein the ZrSi is adopted2The preparation method of the-SiC powder comprises the following steps:
step A, 60 to 90 wt.% of ZrSi2Uniformly mixing 10-40 wt.% of SiC powder by adopting a planetary ball mill wet milling method to obtain mixed powder;
b, mixing and stirring 40-50 wt.% of mixed powder, 6-9 wt.% of binder and 44-51 wt.% of distilled water for 2 hours to obtain mixed slurry;
and C: granulating the mixed slurry by adopting a centrifugal sprayer to obtain spherical ZrSi2-SiC powder.
6. The method for preparing the C/C composite material surface oxidation resistant coating as claimed in claim 5, wherein the inlet temperature of the centrifugal spraying machine is 280-320 ℃, and the outlet temperature is 110-140 ℃.
7. The preparation method of the C/C composite material surface oxidation resistant coating according to claim 1, characterized in that the specific process of the step 2 is as follows: ZrSi is sprayed by adopting a supersonic plasma spraying method2Spraying SiC powder on the surface of the C/C composite material protected by the SiC coating to obtain ZrSi on the surface of the C/C composite material2-SiC/SiC oxidation resistant coating.
8. The preparation method of the C/C composite material surface oxidation resistant coating according to claim 7, characterized in that the technological parameters of the supersonic plasma spraying method are as follows: the power is 30-50KW, the Ar flow is 65-80L/min, the powder feeding amount is 10-40g/min, and the spraying distance is 80-120 mm.
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