CN112501613B - Full-temperature-range oxidation-resistant ablative coating and preparation method thereof - Google Patents
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- C23C28/341—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one carbide layer
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
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Abstract
The invention relates to a full-temperature-range oxidation-resistant ablation coating and a preparation method thereof, wherein the coating comprises a SiC transition layer and an oxidation-resistant ablation coating, wherein the SiC transition layer and the oxidation-resistant ablation coating are sequentially formed on a base material; in ZrB 2 、MoSi 2 ZrB in doped W oxidation resistant ablative coatings 2 Is 10-20% of MoSi 2 The mass percentage of the components is 10-20%. The preparation method comprises preparing SiC transition layer by chemical vapor deposition; zrB preparation by adopting atmospheric plasma spraying method 2 、MoSi 2 Doped W coating. The full-temperature-range ablation-resistant coating has a full-temperature-range glass phase with a high temperature of more than 3000 ℃ from room temperature, the high temperature resistance of the tungsten coating is taken as ablation resistance, the ceramic glass phase prevents oxidizing atmosphere from migrating into the material through cracks and pores, the service time of ablation resistance of the coating in the full-temperature range is prolonged, and the coating has an effective protection effect on a matrix composite material; the full-temperature-range ablation-resistant coating has the advantages of compact structure, small porosity, high bonding strength, full-temperature-range ablation resistance and the like.
Description
Technical Field
The invention belongs to the technical field of high-temperature ablative coatings, and particularly relates to a full-temperature-range antioxidant ablative coating and a preparation method thereof.
Background
The hypersonic flight technology and the solid rocket engine technology are core technologies in the aerospace field and are also key development technologies in various aerospace major countries in recent years. The hypersonic flight generates pneumatic heating, ablative components such as a throat insert and a nozzle of the solid rocket engine are subjected to high temperature of fuel gas, and the temperature of the components such as a front edge, a nose cone and the nozzle generally exceeds thousands of degrees or even reaches thousands of degrees in work. Under the condition, the harsh extreme conditions of oxidation resistance, ablation resistance, particle erosion resistance and the like from room to more than 3000 ℃ are difficult to meet only depending on the performance of composite materials such as C/C, C/SiC, C/C-SiC and the like, and an oxidation and ablation resistant coating needs to be coated on the surface of the material.
Tungsten (W) is metal with the highest melting point (about 3420 ℃), has the advantages of good high-temperature performance, high thermal conductivity, low thermal expansion coefficient, thermal shock resistance, ablation resistance and the like, is used as a high-temperature ablation resistant material such as a throat liner of a solid rocket engine and the like, but has the problems of low structural strength, high density, large inert mass and oxidation after the temperature exceeds 1400 ℃, and the tungsten is used as a coating, so that the quality is not obviously increased, the ablation resistance of the material in a short time is improved, and the tungsten is one of candidate materials for a high-temperature ablation resistant coating in the aerospace field.
At present, the preparation technology of the oxidation-resistant ablative coating mainly comprises an embedding reaction method, a slurry brushing method, plasma spraying, physical vapor deposition, chemical vapor deposition, magnetron sputtering and the like. The plasma spraying method has simple process and low cost, is not limited by the size and the shape of a workpiece, can repair a coating, and is the most common engineering method. However, the existing plasma spraying coating mainly has the problem of large porosity, the oxidation and ablation resistant coating material mainly comprises a series of ceramic coatings of carbide, boride and silicon-containing compounds, the problems of multiple process links, long period, high cost and the like mainly exist, key technologies such as interface compatibility, thermal expansion matching, high temperature stability and the like are not thoroughly solved, and accurate control and engineering are not easy to realize.
Disclosure of Invention
The invention provides a full-temperature-range anti-oxidation ablative coating and a preparation method thereof, and solves the problems of long preparation period, high cost, small use temperature range and difficult realization of engineering in the existing high-temperature anti-ablation coating technology.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the full-temperature-range oxidation-resistant ablative coating comprises a SiC transition layer and an oxidation-resistant ablative coating which are sequentially formed on a base material, wherein the oxidation-resistant ablative coating is formed by ZrB 2 、MoSi 2 And W.
Further, zrB in the oxidation-resistant ablative coating 2 Is 10-20% of MoSi 2 The mass percentage of the components is 10-20%; the mass percentage of W is more than 60 percent.
Furthermore, the thickness of the SiC transition layer is 20-50 μm.
Further, the thickness of the oxidation ablation resistant coating is 200-500 μm.
A preparation method of a full-temperature-range oxidation and ablation resistant coating comprises the following steps:
step 1, preparing a SiC transition layer on the surface of a base material by adopting a chemical vapor deposition method;
step 2, preparing ZrB on the SiC transition layer by adopting an atmospheric plasma spraying method 2 、MoSi 2 Doped W resists oxidative ablation of the coating.
Further, the step 1 comprises the following steps:
101, carrying out ultrasonic cleaning treatment on a base material;
102, drying the base material at 80-100 ℃ for 4-6 h;
and 103, depositing for 5 to 20 hours at the temperature of 1100 to 1300 ℃ by taking methyltrichlorosilane as a raw material, hydrogen as a carrier gas and nitrogen as a diluent gas to obtain the SiC transition layer with the thickness of 20 to 50 mu m.
Further, the step 2 comprises the following steps:
step 201. The mass percent is 10-20% 2 Powder with the mass percent of 10-20 percent of MoSi 2 Mixing the powder with 60-80 wt% of powder, and loading into powder feeder for plasma spraying;
202, fixing the matrix material with the SiC transition layer in the step 1 on a spraying platform;
step 203, preparing ZrB by adopting atmospheric plasma spraying 2 、MoSi 2 A doped W oxidation ablation resistant coating; in the spraying process, argon is used as main gas, and the flow rate is 50l/min; hydrogen is used as auxiliary gas, and the flow rate is 7l/min; nitrogen is used as powder feeding gas, the voltage is 50-60V, the current is 600-700A, the spraying distance is 100-150 mm, the powder feeding speed is 10-30 g/min, and the thickness of the coating is 200-500 mu m.
Further, zrB in step 201 2 Powder, moSi 2 The particle size of the powder is 10-40 μm, and the particle size of the W powder is 20-70 μm.
Compared with the prior art, the invention has the beneficial effects that:
(1) The full-temperature-range oxidation-resistant ablative coating adopts a chemical vapor deposition SiC transition layer, the purity of the transition layer is high, the quality is good, the high-temperature stability is good (CVD SiC is thermally decomposed at 2700 ℃), and the bonding strength reduction caused by the mutual diffusion reaction between the W coating and the matrix material is prevented; secondly, the SiC transition layer relieves the thermal stress between the coating and the base material caused by the mismatching of the thermal expansion coefficients;
(2) ZrB for doping in the invention 2 、MoSi 2 The powder has a melting point lower than that of W powder, and can well fill the defects of interlayer micro holes, gaps and the like of the W coating in the spraying process, improve the density of the W coating, and block an oxidation component H 2 O、O 2 Channels for isotropic coating and matrix diffusion;
(3) ZrB for doping in the invention 2 、MoSi 2 In the powder, at the temperature below 1000 ℃, B element reacts with oxygen to generate glassy B 2 O 3 The oxidation resistance of the W coating is improved by sealing and filling cracks and pores generated in the oxidation and ablation processes; si element reacts with oxygen to generate glassy SiO in the temperature range of 1000-2000 DEG C 2 The molten W coating is melted and flows, so that cracks and pores generated in the oxidation and ablation processes are sealed and healed, and the oxidation resistance of the W coating is improved; zr element reacts with oxygen to generate glass-state ZrO at the temperature of more than 2000 DEG C 2 The melting and flowing are adopted to seal and heal cracks and pores generated in the oxidation and ablation processes, so that the oxidation and ablation resistance of the W coating is improved; the global anti-oxidation ablation from room temperature to ultrahigh temperature is realized;
(4) The chemical vapor deposition process and the plasma spraying process can be used for quickly and efficiently preparing the high-performance coating which is antioxidant and ablation-resistant on the surface of a substrate material (such as a ceramic substrate) at low cost. The chemical vapor deposition time is short, the temperature is low, and the obtained SiC has high quality and good performance; the used atmospheric plasma spraying process is simple, has low requirements on equipment and low cost, is suitable for parts with complex shapes, has unlimited size and is convenient for large-scale industrial application.
Drawings
FIG. 1 is a surface macro topography of a full temperature range oxidation ablation resistant coating prepared on a substrate in example 1 of the present invention;
FIG. 2 is a surface micro-topography of a full-temperature-range oxidation-ablation-resistant coating prepared on a substrate in example 1 of the present invention;
FIG. 3 is a cross-sectional backscatter view of a full temperature range oxidation resistant ablative coating prepared on a substrate in example 1 of the present invention;
FIG. 4 is a schematic view of the structure of the full-temperature-range anti-oxidation ablative coating of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the present invention will be described in further detail with reference to embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a full-temperature-range oxidation-resistant ablative coating and a preparation method thereof, the full-temperature-range oxidation-resistant ablative coating comprises a SiC transition layer and an oxidation-resistant ablative coating which are sequentially formed on a substrate material, and the oxidation-resistant ablative coating is formed by ZrB 2 (zirconium boride), moSi 2 A (molybdenum disilicide) doped W (tungsten) coating, see fig. 4. The SiC transition layer mainly has the functions of preventing the mutual diffusion reaction between the W coating and the matrix material from causing the reduction of the bonding strength and relieving the thermal stress generated by the mismatching of the thermal expansion coefficients between the coating and the matrix; the temperature range below 1000 ℃ mainly depends on the oxidation resistance and the ablation resistance of W, and the B element in the coating can react with oxygen to generate glassy B 2 O 3 The coating can seal and fill cracks and pores generated in the oxidation and ablation processes, and improve the oxidation resistance and the ablation resistance of the W coating; in the temperature range of 1000-2000 deg.c, the Si element in the coating reacts with oxygen to produce glass SiO 2 Melting and flowing, oxidizing and burningCracks and pores generated in the etching process are sealed and filled, so that the oxidation resistance and the ablation resistance of the W coating are improved; the glass state ZrO can be generated at the temperature of more than 2000 ℃ mainly by the reaction of Zr element in the coating and oxygen 2 Melting and flowing, sealing and filling cracks and pores generated in the oxidation and ablation processes, and improving the oxidation and ablation resistance of the W coating; the coating prepared by the invention has the advantages of compact structure, small porosity, high bonding strength, ablation resistance in the full temperature range, excellent performance and the like.
Two specific examples of the preparation method of the full-temperature-range oxidation-resistant ablative coating of the invention are described below.
Example 1:
a preparation method of a full-temperature-range oxidation and ablation resistant coating comprises the following steps:
step 1, preparing the SiC transition layer on the surface of a base material by adopting a chemical vapor deposition method;
step 2, preparing ZrB on the substrate with the SiC transition layer by adopting an atmospheric plasma spraying method 2 、MoSi 2 And (3) the doped W is resistant to oxidation and ablation, so that the full-temperature-range anti-oxidation and ablation coating is formed on the substrate.
Step 1 comprises the following substeps:
101, performing ultrasonic cleaning treatment on a base material in distilled water for 2 hours;
102, drying the base material at 100 ℃ for 4 hours;
and 103, depositing for 10 hours at 1100 ℃ by taking Methyl Trichlorosilane (MTS) as a raw material, hydrogen as a carrier gas and nitrogen as a diluent gas to obtain the SiC transition layer with the thickness of 20 microns.
Step 2 comprises the following substeps:
step 201, zrB with the mass percent of 10% 2 Powder, mass percent 20% MoSi 2 The powder is uniformly mixed with 70 percent of W powder by mass percent and then is put into a powder feeder for plasma spraying; zrB 2 Powder, moSi 2 The particle size of the powder is 10-40 μm, and the particle size of the W powder is 20-70 μm;
step 202, fixing the base material with the SiC transition layer in the step 1 on a spraying platform;
step 203, preparing ZrB by adopting atmospheric plasma spraying 2 、MoSi 2 The doped W coating is sprayed by taking argon as main gas and the flow rate is 50l/min; hydrogen is used as auxiliary gas, and the flow rate is 7l/min; the nitrogen is used as powder feeding gas, the voltage is 50V, the current is 600A, the spraying distance is 100mm, the powder feeding speed is 20g/min, and the thickness of the obtained coating is 200 mu m;
referring to fig. 1, the macro topography of the surface of the full-temperature-range oxidation-resistant ablative coating prepared on the substrate according to the present example; referring to fig. 2, the micro-topography of the surface of the full-temperature-range oxidation-resistant ablative coating prepared on the substrate according to the present example; referring to fig. 3, this example is a cross-sectional backscatter plot of the full temperature range oxidation resistant ablative coating prepared on a substrate.
The full-temperature-range oxidation-resistant ablation coating prepared by the implementation is subjected to flame ablation examination of oxyacetylene at the temperature of 2200 ℃, the coating can protect a substrate material from oxidation and ablation for 180s, and the surface of the substrate is not exposed.
Example 2:
a preparation method of a full-temperature-range oxidation and ablation resistant coating comprises the following steps:
step 1, preparing the SiC transition layer on the surface of a base material by adopting a chemical vapor deposition method;
step 2, preparing ZrB on the substrate with the SiC transition layer by adopting an atmospheric plasma spraying method 2 、MoSi 2 And (3) the doped W is resistant to oxidation and ablation, so that the full-temperature-range anti-oxidation and ablation coating is formed on the substrate.
Step 1 comprises the following substeps:
101, carrying out ultrasonic cleaning treatment on a base material in distilled water for 4 hours;
102, drying the base material for 6 hours at the temperature of 80 ℃;
and 103, depositing for 20 hours at 1300 ℃ by using Methyl Trichlorosilane (MTS) as a raw material, hydrogen as a carrier gas and nitrogen as a diluent gas to obtain the SiC transition layer, wherein the thickness of the coating is 50 microns.
Step 2 comprises the following substeps:
step 201, zrB with the mass percent of 20% 2 Powder, mass percent is 10 percent MoSi 2 Uniformly mixing the powder with 70% of W powder by mass percent, and filling the mixture into a powder feeder for plasma spraying; zrB 2 Powder, moSi 2 The particle size of the powder is 10-40 μm, and the particle size of the W powder is 20-70 μm;
202, fixing the base material with the SiC transition layer in the step 1 on a spraying platform;
step 203, preparing ZrB by adopting atmospheric plasma spraying 2 、MoSi 2 The doped W coating is sprayed by taking argon as main gas and the flow rate is 50l/min; hydrogen is used as auxiliary gas, and the flow rate is 7l/min; the nitrogen is used as powder feeding gas, the voltage is 60V, the current is 700A, the spraying distance is 150mm, and the powder feeding speed is 30g/min. The thickness of the coating was 500. Mu.m;
the coating is subjected to plasma flame ablation examination at the temperature of about 5000 ℃, can protect the substrate material from resisting oxidation ablation for 30s, and does not expose the surface of the substrate.
The present invention has been described in terms of specific examples, which are provided to aid in understanding the invention and are not intended to be limiting. Any partial modification or replacement of the present invention by a person skilled in the art within the technical scope of the present invention should be covered within the scope of the present invention.
Claims (5)
1. A preparation method of a full-temperature-range oxidation and ablation resistant coating is characterized by comprising the following steps:
the oxidation-resistant ablative coating comprises a SiC transition layer and an oxidation-resistant ablative layer which are sequentially formed on a base material, wherein the oxidation-resistant ablative layer is formed by ZrB 2 、MoSi 2 And W;
ZrB in the oxidation resistant ablative layer 2 Is 10-20% of MoSi 2 The mass percent of the W is 10-20%, and the mass percent of the W is more than 60%;
the preparation method of the full-temperature-range oxidation and ablation resistant coating comprises the following steps:
step 1, preparing a SiC transition layer on the surface of a base material by adopting a chemical vapor deposition method;
step 2, preparing the oxidation-resistant ablation layer on the SiC transition layer by adopting an atmospheric plasma spraying method;
the step 1 comprises the following steps:
101, carrying out ultrasonic cleaning treatment on a base material;
102, drying the base material at the temperature of 80-100 ℃ for 4-6 h;
and 103, depositing for 5 to 20h at the temperature of 1100 to 1300 ℃ by taking methyltrichlorosilane as a raw material, hydrogen as a carrier gas and nitrogen as a diluent gas to obtain a SiC transition layer with the thickness of 20 to 50 mu m.
2. The method for preparing the full-temperature-range oxidation and ablation resistant coating according to claim 1, characterized in that: the thickness of the SiC transition layer is 20 to 50 mu m.
3. The method for preparing the full-temperature-range oxidation-resistant ablative coating according to claim 2, characterized in that: the thickness of the oxidation-resistant ablation layer is 200-500 mu m.
4. The preparation method of the full-temperature-range oxidation and ablation resistant coating according to claim 3, characterized by comprising the following steps: the step 2 comprises the following steps:
step 201, zrB with the mass percentage of 10-20% 2 Powder of 10-20% MoSi by mass 2 Uniformly mixing the powder with 60-80% of W powder by mass percent, but not including 60% of W powder at the end point, and filling the mixture into a powder feeder for plasma spraying;
step 202, fixing the matrix material with the SiC transition layer in the step 1 on a spraying platform;
step 203, preparing ZrB by adopting atmospheric plasma spraying 2 、MoSi 2 A doped W oxidation resistant ablative layer; in the spraying process, argon is used as main gas, and the flow is 50L/min; hydrogen is used as auxiliary gas, and the flow rate is 7L/min; nitrogen is used as powder feeding gas, the voltage is 50-60V, the current is 600-700A, the spraying distance is 100-150mm, the powder feeding speed is 10-30g/min, and the coating thickness is 200-500μm。
5. The method for preparing the full-temperature-range oxidation-resistant ablative coating of claim 4, wherein the method comprises the following steps: zrB in step 201 2 Powder, moSi 2 The particle size of the powder is 10-40 mu m, and the particle size of the W powder is 20-70 mu m.
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