CN114315390A - Carbon/carbon composite material surface wide-temperature-range long-life antioxidant coating and low-temperature preparation method - Google Patents
Carbon/carbon composite material surface wide-temperature-range long-life antioxidant coating and low-temperature preparation method Download PDFInfo
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Abstract
The invention relates to a wide-temperature-range long-life antioxidant coating on the surface of a carbon/carbon composite material and a low-temperature preparation method, which are used for improving the antioxidant performance of the C/C composite material in a wide temperature range (900-1500 ℃). The technical scheme of the invention is that a porous HfB is prepared on the surface of a C/C composite material coated with SiC by a cold coating method2-SiC precoat, then subjecting the precoat to a low temperature densification treatment to bring about HfB2In situ generation of B2O3The glass fills the pores and the ceramic particles in the bond coat to form a porous B-rich coating2O3Glass, SiC and HfO2Composite coatings of ceramic particles. Under the low and medium temperature oxidation environment, the coating can generate borosilicate glass and SiO respectively2Glass, as an oxygen barrier to protect the C/C composite from oxidation. In addition, Hf-oxides (HfO) in the coating2And HfSiO4) The ceramic particles can toughen the glass and inhibit the volatilization of the glass. Therefore, the coating can protect the C/C composite material from long-life oxidation within a wide temperature range of 900-1500 ℃.
Description
Technical Field
The invention belongs to the field of carbon/carbon composite material antioxidant coatings, and relates to a wide-temperature-range long-life antioxidant coating on the surface of a carbon/carbon composite material and a low-temperature preparation method.
Background
The carbon/carbon (C/C) composite material is an ultra-high temperature thermal structure material which is composed of carbon fibers and a carbon matrix and has excellent high-temperature mechanical properties, and has great potential to be applied to the field of aerospace. However, the C/C composite material is easily oxidized in an aerobic environment at the temperature higher than 450 ℃ to cause damage to a carbon matrix and carbon fibers, so that the mechanical property of the C/C composite material is greatly reduced, and the application of the material in the field of ultrahigh temperature is limited. In order to improve the high-temperature oxidation resistance of the C/C composite material, matrix modification and surface coating technologies are developed by extensive researchers, wherein the surface coating can be used for blocking the contact of oxygen and the C/C composite material, so that the preparation of the oxidation resistant coating is an effective means for realizing long-time protection of the C/C composite material. The oxidation resistant coating commonly used at present is a silicon-based ceramic coating, because the coating can generate a layer of compact SiO on the surface when being oxidized at high temperature (1400-1600 ℃), and2the glass layer can heal micro cracks in the coating, and effectively hinders the diffusion of oxygen to the C/C composite material matrix. However, when the oxidation temperature is lower than 1200 ℃, the oxidation rate of the silicon-based ceramic coating is very low, and SiO is generated in a short time2Glass is few and has high viscosity, and the cracks are difficult to effectively heal. In order to improve the protection capability of the silicon-based ceramic coating on the C/C composite material at medium and low temperatures, document 1 "q.g.fu, h.j.li, y.j.wang, k.z.li, x.h.shi, B2O3 modified SiC-MoSi2oxidation resistance coating for carbon/carbon composites by a two-step pack compensation, coros. Sci.51(2009)2450-The introduction of B by embedding into B was proposed for both the ilayer and multi-component oxidation protective coating system for carbon/carbon components from the room temperature to 1873K, Corros Sci.72(2013)144-1492O3Modified silicon-based ceramic coatings because of B at 900 deg.C2O3Glass to SiO2The glass has lower viscosity and can be mixed with SiO2The generation of borosilicate glass which heals microcracks in silicon-based ceramic coatings, so that B is comparable to silicon-based ceramic coatings2O3The modified silicon-based ceramic coating obtains better oxidation resistance under the oxidation environment of 900 ℃. However, the preparation temperature required for preparing the coating by the embedding method is more than 1900 ℃, the holding time is 1 to 3 hours, and at the high temperature and the long time, the B with low melting point and high vapor pressure in the embedded powder2O3Will volatilize rapidly, leading to B in the coating obtained by the preparation method2O3The content is low, and the effective protection time of the coating at 900 ℃ is only 150 h. Thus B prepared by high temperature embedding2O3The modified silicon-based ceramic coating can not meet the requirement of a long-life protective C/C composite material. Document 3 discloses a method for preparing a SiC-Si/TiB by combining slurry dip coating and gas phase siliconizing (CN113716977A)2-SiC-Si/SiC-Si/SiO2-B multilayer composite oxidation resistant coating. In the preparation method, the gas-phase siliconizing temperature is higher (more than or equal to 1800 ℃), in addition, the coating system is composed of four layers of coatings, the preparation steps are complicated, the process is complex, uncontrollable factors are more, the cost is high, the coating is weightless even under the condition of only protecting the C/C composite material for 182h at 900 ℃, the obtaining effect is limited, and the long-life protection of the C/C composite material cannot be realized. In view of the high preparation temperature of the coating, B in the coating2O3The content is low, the protection time is short, and a coating which can realize long-life oxidation resistance in a wide temperature range needs to be prepared at low temperature.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention providesThe surface wide-temperature-range long-life antioxidant coating of the carbon/carbon composite material and the low-temperature preparation method solve the problem of high preparation temperature of the wide-temperature-range antioxidant coating, and can further realize that the coating can protect the long-life antioxidant property of the C/C composite material. Firstly, a cold coating method is adopted to prepare a porous HfB2And (2) preparing a SiC precoat, and finally preparing the long-life antioxidant coating on the surface of the C/C composite material in a wide-temperature-range atmospheric environment at the temperature of 900-1500 ℃ by carrying out low-temperature densification treatment on the precoat.
Technical scheme
A carbon/carbon composite material surface oxidation resistant coating with wide temperature range and long service life is characterized in that the coating is composed of B2O3Glass, HfO2And SiC ceramic particles, wherein the glass and the ceramic particles are embedded and compounded with each other; b is2O3Glass is used as a binder to be filled among the ceramic particles to bond the ceramic particles together; the surface oxidation resistant coating of the C/C composite material is used in a wide temperature range of 900-1500 ℃.
A method for preparing the anti-oxidation coating with wide temperature range and long service life on the surface of the carbon/carbon composite material at low temperature is characterized by comprising the following steps:
step 1: HfB with the mass percentage of 20-90 percent2Adding the powder and 10-80% of SiC powder into 1-10 wt% polyvinyl butyral PVB alcohol solution, and fully stirring under a magnetic stirrer to obtain slurry;
step 2: placing the C/C composite material with the SiC coating on the surface into slurry for cold coating, and taking out after immersing for 1-3 seconds;
and step 3: repeating the step 2 for 10-20 times, and drying and curing the C/C composite material with the coating in an oven at 50-80 ℃ to obtain porous HfB on the surface of the C/C composite material2-a pre-coating of SiC;
and 4, step 4: will have porous HfB2And (3) placing the C/C composite material coated with the-SiC precoat in a 900-1200 ℃ heat treatment furnace, and performing densification treatment on the C/C composite material for 5-30 mins in an atmospheric environment to finally prepare the anti-oxidation coating with wide temperature range and long service life on the surface of the C/C composite material.
The HfB2Particle size of the powder: d50＝2.0μm。
The granularity of the SiC powder is as follows: d50＝6.5μm。
And (3) fully stirring in the step (1) for 2-4 h.
Advantageous effects
The invention provides a wide-temperature-range long-life antioxidant coating on the surface of a carbon/carbon composite material and a low-temperature preparation method, which are used for improving the antioxidant performance of the C/C composite material in a wide temperature range (900-1500 ℃). The technical scheme of the invention is that a porous HfB is prepared on the surface of a C/C composite material coated with SiC by a cold coating method2-SiC precoat, then subjecting the precoat to a low temperature densification treatment to bring about HfB2In situ generation of B2O3The glass fills the pores and the ceramic particles in the bond coat to form a porous B-rich coating2O3Glass, SiC and HfO2Composite coatings of ceramic particles. Under the low and medium temperature oxidation environment, the coating can generate borosilicate glass and SiO respectively2Glass, as an oxygen barrier to protect the C/C composite from oxidation. In addition, Hf-oxides (HfO) in the coating2And HfSiO4) The ceramic particles can toughen the glass and inhibit the volatilization of the glass. Therefore, the coating can protect the C/C composite material from long-life oxidation within a wide temperature range of 900-1500 ℃.
1) The preparation temperature of other anti-oxidation coatings with wide temperature ranges is above 1800 ℃, the preparation temperature of the coating preparation method is reduced to below 1200 ℃, so that the thermal stress generated by the difference of thermal expansion coefficients between the coating and the matrix is reduced, and the cracking of the coating is effectively inhibited;
2) b in other coatings2O3Or B is introduced externally and in a lower amount, the porous HfB of the present invention2the-SiC precoat passes through HfB during densification2Preoxidation in situ generation of large amounts of B2O3Glass filled in the micropores of the coating layer to make the B in the wide temperature range oxidation resistant coating layer2O3The content is obviously improved;
3) compared with other glass layers with ceramic coating surfaces easy to crack, B2O3The glass is embedded among the ceramic particles, which is favorable for inhibitingThe prepared glass is cracked, so the glass-ceramic mosaic structure in the coating has better capability of blocking oxygen diffusion;
4) b in the coating during low-temperature oxidation2O3Glass hinders oxygen diffusion, SiO generated in situ by SiC during high-temperature oxidation2The glass continues to play the role of oxygen resistance, so the coating can protect the C/C composite material at 900 ℃, 1200 ℃ and 1500 ℃ for the oxidation resistance time of 403 hours, 723 hours and 403 hours respectively.
Drawings
FIG. 1 is a flow chart of the method for preparing the anti-oxidation coating with wide temperature range and long service life at low temperature;
FIG. 2 is a wide temperature range long life oxidation resistant coating prepared by method example 3 of the present invention: (a) coating the surface; (b) coating XRD pattern; (c) coating cross section; (d) local enlargement of the cross section; (e) scanning results of EDS energy spectrum points;
FIG. 3 is a graph showing the oxidation resistance of a coated sample prepared by the method of example 3 of the present invention in a wide temperature range;
FIG. 4 is a cross-section of a high temperature produced coating of example 1 of the process of the present invention;
FIG. 5 shows an example of a method of the present invention, example 2 Low HfB2The cross section of the coating prepared by the method.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1:
weighing 2g HfB2Powder (particle size: D)502.0 μm) and 8g of SiC powder (particle size: d506.5 μm), added to 30ml of a 1 wt.% PVB alcoholic solution and stirred well for 2 hours with a magnetic stirrer. And (3) carrying out cold coating on the C/C composite material with the SiC coating on the surface in the slurry, and taking out after immersing for 1-3 seconds. After continuously repeating cold coating for 10 times, the carbon/carbon composite material with the coating is put into a 50 ℃ oven for drying and curing to obtain porous HfB2-a pre-coating of SiC. Porous HfB2Putting the carbon/carbon composite material coated with the-SiC precoat layer into a 900 ℃ heat treatment furnace, performing 5mins densification in the atmospheric environment, and finally preparing the wide area on the surface of the C/C composite materialA long-life antioxidant coating in a temperature range.
Example 2:
weighing 3g HfB2Powder (particle size: D)502.0 μm) and 7g of SiC powder (particle size: d506.5 μm), added to 40ml of a 2 wt.% PVB alcoholic solution and stirred thoroughly for 3 hours with a magnetic stirrer. And (3) carrying out cold coating on the C/C composite material with the SiC coating on the surface in the slurry, and taking out after immersing for 1-3 seconds. After continuously repeating cold coating for 15 times, the C/C composite material with the coating is put into a 60 ℃ oven for drying and curing to obtain porous HfB2-a pre-coating of SiC. Porous HfB2Putting the C/C composite material coated with the-SiC precoat in a 1000 ℃ heat treatment furnace, and performing densification for 10mins in an atmospheric environment to finally prepare the anti-oxidation coating with wide temperature range and long service life on the surface of the C/C composite material.
Example 3:
weighing 5g HfB2Powder (particle size: D)502.0 μm) and 5g of SiC powder (particle size: d506.5 μm), added to 50ml of an 8 wt.% strength alcoholic PVB solution and stirred thoroughly for 4 hours with a magnetic stirrer. And (3) carrying out cold coating on the C/C composite material with the SiC coating on the surface in the slurry, and taking out after immersing for 1-3 seconds. After continuously repeating cold coating for 20 times, the C/C composite material with the coating is put into an oven at 70 ℃ for drying and curing to obtain porous HfB2-a pre-coating of SiC. Porous HfB2Putting the C/C composite material coated with the-SiC precoat in a 1100 ℃ heat treatment furnace, and performing densification for 30mins in an atmospheric environment to finally prepare the anti-oxidation coating with wide temperature range and long service life on the surface of the C/C composite material.
Example 1, the preparation temperature was increased to 1500 ℃:
weighing 5g HfB2Powder (particle size: D)502.0 μm) and 5g of SiC powder (particle size: d506.5 μm), added to 50ml of an 8 wt.% strength alcoholic PVB solution and stirred thoroughly for 4 hours with a magnetic stirrer. And (3) carrying out cold coating on the C/C composite material with the SiC coating on the surface in the slurry, and taking out after immersing for 1-3 seconds. After continuously repeating cold coating for 20 times, placing the C/C composite material with the coatingDrying and curing in a 70 ℃ oven to obtain porous HfB2-a pre-coating of SiC. Porous HfB2Putting the C/C composite material coated with the-SiC precoat in a 1500 ℃ heat treatment furnace, and performing densification for 30mins in an atmospheric environment to finally prepare the anti-oxidation coating with wide temperature range and long service life on the surface of the C/C composite material.
Example 2, HfB2The powder content is reduced to below 20 wt.% by mass:
weighing 1g HfB2Powder (particle size: D)502.0 μm) and 9g of SiC powder (particle size: d506.5 μm), added to 50ml of an 8 wt.% strength alcoholic PVB solution and stirred thoroughly for 4 hours with a magnetic stirrer. And (3) carrying out cold coating on the C/C composite material with the SiC coating on the surface in the slurry, and taking out after immersing for 1-3 seconds. After continuously repeating cold coating for 20 times, the C/C composite material with the coating is put into an oven at 70 ℃ for drying and curing to obtain porous HfB2-a pre-coating of SiC. Porous HfB2Putting the C/C composite material coated with the-SiC precoat in a 1100 ℃ heat treatment furnace, and performing densification for 30mins in an atmospheric environment to finally prepare the anti-oxidation coating with wide temperature range and long service life on the surface of the C/C composite material.
FIG. 1 is a flow chart of the low-temperature preparation of the wide-temperature-range long-life oxidation-resistant coating, and the maximum temperature of the coating prepared by the method is only 1200 ℃, which is far lower than the preparation temperature of the wide-temperature-range oxidation-resistant coating obtained by other methods. FIG. 2 shows the microstructure and phase composition of a wide temperature range long life oxidation resistant coating prepared at low temperature. As can be seen from FIG. 2a, the coating surface is dense and no cracks are generated due to the low temperature preparation. The surface of the coating is composed of a plurality of nanometer white particles and a glass phase. As can be seen from an XRD pattern, the coating mainly has an amorphous glass phase (steamed bread peak near 20 degrees), crystalline SiC and HfO2And (4) forming. The coating section is composed of an inner coating silicon carbide and an outer coating. From the local enlargement of the overcoat layer, the black phase, the gray phase and the white phase are B respectively in combination with the dot-scan EDS structure2O3Glass, slightly oxidized SiC and HfO2Ceramic particles. Wherein B is2O3The glass is HfB in a pre-coating during densification2The oxidation is generated in situ, and the oxidation is carried out,filled between ceramic particles, and finally obtaining a glass-ceramic composite coating through low-temperature densification. FIG. 3 is an oxidation resistance curve diagram of a coating sample at 900-1500 ℃, and it can be seen that the coating can protect carbon-carbon composite materials at 900 ℃, 1200 ℃ and 1500 ℃ for oxidation resistance times of 403 hours, 723 hours and 403 hours, respectively, and achieve the performance targets of wide temperature range and long life oxidation resistance. FIG. 4 is a reverse example of the design of the present invention, i.e., the high temperature preparation of the coating cross-sectional profile, and it can be seen that there are many bubbles in the coating due to HfB densification at 1500 deg.C2Violent oxidation to form B2O3The glass rapidly volatilizes, generating a large amount of bubbles, seriously damaging the integrity of the coating. FIG. 5 is a reverse example of the design of the present invention, namely a low HfB content2The cross-sectional shape of the coating after being densified is due to HfB2Low content of B produced during densification2O3Less glass is not enough to fully densify the coating, so a large number of holes are present in the coating.
Claims (5)
1. A carbon/carbon composite material surface oxidation resistant coating with wide temperature range and long service life is characterized in that the coating is composed of B2O3Glass, HfO2And SiC ceramic particles, wherein the glass and the ceramic particles are embedded and compounded with each other; b is2O3Glass is used as a binder to be filled among the ceramic particles to bond the ceramic particles together; the surface oxidation resistant coating of the C/C composite material is used in a wide temperature range of 900-1500 ℃.
2. A method for preparing the anti-oxidation coating with wide temperature range and long service life on the surface of the carbon/carbon composite material as claimed in claim 1 at low temperature is characterized by comprising the following steps:
step 1: HfB with the mass percentage of 20-90 percent2Adding the powder and 10-80% of SiC powder into 1-10 wt% polyvinyl butyral PVB alcohol solution, and fully stirring under a magnetic stirrer to obtain slurry;
step 2: placing the C/C composite material with the SiC coating on the surface into slurry for cold coating, and taking out after immersing for 1-3 seconds;
and step 3: repeating the step 2 for 10-20 times, and drying and curing the C/C composite material with the coating in an oven at 50-80 ℃ to obtain porous HfB on the surface of the C/C composite material2-a pre-coating of SiC;
and 4, step 4: will have porous HfB2And (3) placing the C/C composite material coated with the-SiC precoat in a 900-1200 ℃ heat treatment furnace, and performing densification treatment on the C/C composite material for 5-30 mins in an atmospheric environment to finally prepare the anti-oxidation coating with wide temperature range and long service life on the surface of the C/C composite material.
3. The method of claim 2, wherein: the HfB2Particle size of the powder: d50＝2.0μm。
4. The method of claim 2, wherein: the granularity of the SiC powder is as follows: d50＝6.5μm。
5. The method of claim 2, wherein: and (3) fully stirring in the step (1) for 2-4 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116639980A (en) * | 2023-05-22 | 2023-08-25 | 中南大学 | Preparation method of multi-carbide ceramic coating |
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