Anti-corrosion and radar-infrared compatible stealth function integrated coating and preparation method thereof
By preparing a layered coating on ceramic matrix composites that integrates corrosion resistance and radar-infrared compatible stealth functions, the corrosion resistance and stealth problems of ceramic matrix composites at ultra-high temperatures were solved, achieving excellent performance above 1400℃.
Patent Information
- Application Number
- CN202511736876.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-25
- Publication Date
- 2026-02-17
- Estimated Expiration
- 2045-11-25
AI Technical Summary
Existing technologies struggle to provide coatings for ceramic matrix composites (CMCs) that simultaneously offer corrosion resistance, radar stealth, and infrared stealth at ultra-high temperatures. In particular, the stealth properties of high-temperature alloy coatings below 1200°C are difficult to directly apply to CMC components.
The coating, which integrates anti-corrosion and radar-infrared compatible stealth functions through a layered structure, includes an adhesive layer, an anti-corrosion layer, a radar absorbing layer, and an infrared stealth layer. It is formed on a ceramic substrate through processes such as atmospheric plasma spraying and suspension plasma spraying. The specific materials include Yb2Si2O7, (Yb0.2Y0.2Er0.2Lu0.2Sc0.2)2Si2O7, La0.7Sr0.3MnO3, Ti3SiC2@YSZ, and precious metal materials.
It achieves excellent corrosion resistance, radar stealth, and infrared stealth effects at ultra-high temperatures. The coating has low infrared emissivity and high radar wave absorption characteristics, and can be effectively used for a long time at temperatures above 1400℃.
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Figure CN121204592B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of metal material plating, in particular to an anti-corrosion and radar-infrared compatible stealth function integrated coating and a preparation method thereof. BACKGROUND
[0002] Aero-engines are developing towards high thrust-to-weight ratio, which inevitably leads to the continuous increase of their working temperature. The surface temperature of the hot end components will exceed 1400℃, which is far beyond the service temperature limit of the existing high-temperature alloy materials. Ceramic matrix composites (CMCs) have low density (about 1 / 3 of high-temperature alloy), high specific strength and specific modulus, and more excellent high-temperature oxidation resistance and creep resistance, with a maximum long-term use temperature of above 1650℃. Therefore, it has become a development trend to replace high-temperature alloys with CMCs to manufacture hot end components (such as tail nozzles, combustion chambers, turbines, etc.) of aero-engines to improve the thrust-to-weight ratio of the engines.
[0003] However, CMCs are prone to water-oxygen corrosion in a high-temperature water vapor environment, which will cause the performance degradation of CMCs and seriously affect their service life. Environmental barrier coating (EBC) is a key means to improve the service reliability of CMCs by protecting CMCs from corrosion. In addition, to meet the demand of the new generation of aircraft for multi-band and all-around stealth capability, CMC components also need to have excellent stealth performance.
[0004] At present, a large number of studies have been carried out on the environmental barrier coating (EBC) for the corrosion resistance of CMCs and some progress has been made, but the related research on stealth coating is still mainly focused on metal substrates. The coating coated on the surface of high-temperature alloy can exhibit stealth performance below 1200℃, which is difficult to be directly applied to CMC components under super-high temperature working conditions.
[0005] Therefore, how to provide an integrated coating for ceramic substrates that has anti-corrosion effect, radar stealth effect and infrared stealth effect at super-high temperature is a current technical difficulty. SUMMARY
[0006] The present application aims to provide an anti-corrosion and radar-infrared compatible stealth function integrated coating and a preparation method thereof to solve the above problems.
[0007] To achieve the above purpose, the present application adopts the following technical solutions:
[0008] An anti-corrosion and radar-infrared compatible stealth function integrated coating, which is arranged on a ceramic substrate.
[0009] The integrated coating comprises a bonding layer, an anti-corrosion layer, a radar wave absorbing layer and an infrared stealth layer arranged in layers, the bonding layer is arranged on the surface of the ceramic substrate;
[0010] The anti-corrosion layer comprises a first sub-anti-corrosion layer, a second sub-anti-corrosion layer and a third sub-anti-corrosion layer arranged in layers, the first sub-anti-corrosion layer is arranged on the surface of the bonding layer;
[0011] The material forming the first sub-anti-corrosion layer comprises Yb2Si2O7 and a first pore-forming agent, the mass of the first pore-forming agent accounts for 15-28% of the total mass of Yb2Si2O7 and the first pore-forming agent;
[0012] The material forming the second sub-anti-corrosion layer comprises (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 and a second pore-forming agent, the mass of the second pore-forming agent accounts for 8-18% of the total mass of (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 and the second pore-forming agent;
[0013] The material forming the third sub-anti-corrosion layer comprises (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7.
[0014] According to the embodiments of the present application, the anti-corrosion layer satisfies at least one of the following conditions:
[0015] (1) the thickness of the anti-corrosion layer is 100-250 μm;
[0016] (2) the thickness of the first sub-anti-corrosion layer is 40-100 μm, the thickness of the second sub-anti-corrosion layer is 40-100 μm, and the thickness of the third sub-anti-corrosion layer is 20-50 μm;
[0017] (3) the porosity of the first sub-anti-corrosion layer is greater than the porosity of the second sub-anti-corrosion layer, and the porosity of the second sub-anti-corrosion layer is greater than the porosity of the third sub-anti-corrosion layer;
[0018] (4) the porosity of the first sub-anti-corrosion layer is 20-30%, and the porosity of the second sub-anti-corrosion layer is 15-25%.
[0019] According to an embodiment of the present application, the adhesive layer satisfies at least one of the following conditions:
[0020] (1) the material forming the adhesive layer comprises Si;
[0021] (2) the thickness of the adhesive layer is 60-110 μm.
[0022] According to an embodiment of the present application, the radar wave absorbing layer satisfies at least one of the following conditions:
[0023] (1) the radar wave absorbing layer comprises a first sub-wave absorbing layer and a second sub-wave absorbing layer arranged in layers, the first sub-wave absorbing layer is arranged on the surface of the corrosion-resistant layer, the material forming the first sub-wave absorbing layer comprises La 0.7 Sr 0.3 MnO3, Al2O3 and SiO2, the material forming the second sub-wave absorbing layer comprises Ti3SiC2@YSZ and Al2O3;
[0024] (2) the thickness of the radar wave absorbing layer is 700-800 μm.
[0025] According to an embodiment of the present application, the radar wave absorbing layer satisfies at least one of the following conditions:
[0026] (1) the thickness ratio of the first sub-wave absorbing layer to the second sub-wave absorbing layer is 5:4-7:3;
[0027] (2) in the material forming the first sub-wave absorbing layer, the mass ratio of the La 0.7 Sr 0.3 MnO3 to the Al2O3 and the SiO2 is (1-3):(2-4):5;
[0028] (3) in the material forming the second sub-wave absorbing layer, the mass of the Ti3SiC2@YSZ accounts for (45-65)% of the mass of the material forming the second sub-wave absorbing layer.
[0029] According to an embodiment of the present application, the area of the orthographic projection of the infrared stealth layer on the radar wave absorbing layer is less than the area of the radar wave absorbing layer, and the orthographic projection of the infrared stealth layer on the radar wave absorbing layer is a plurality of array-arranged squares;
[0030] The side length of the square is 0.8-3.5 mm, and the interval distance between adjacent squares is 0.5-1.2 times the side length of the square.
[0031] According to an embodiment of the present application, the infrared stealth layer satisfies at least one of the following conditions:
[0032] (1) the material forming the infrared stealth layer comprises Ti3SiC2 and a noble metal material, the noble metal material comprises at least one of AgPd, Pt and Pd, and the mass of the noble metal material accounts for 60-80% of the mass of the material forming the infrared stealth layer;
[0033] (2) the thickness of the infrared stealth layer is 20-50 μm.
[0034] The application further provides a preparation method of the corrosion-resistant and radar-infrared compatible stealth function integrated coating as described above, comprising the following steps:
[0035] a bonding layer is formed on the surface of the ceramic substrate by means of atmospheric plasma spraying;
[0036] a first sub-corrosion-resistant layer and a second sub-corrosion-resistant layer are formed on the surface of the bonding layer by means of atmospheric plasma spraying, and a third sub-corrosion-resistant layer is formed on the surface of the second sub-corrosion-resistant layer by means of suspension plasma spraying, and the first sub-corrosion-resistant layer, the second sub-corrosion-resistant layer and the third sub-corrosion-resistant layer constitute a corrosion-resistant layer;
[0037] a radar wave-absorbing layer is formed on the surface of the corrosion-resistant layer;
[0038] an infrared stealth layer is formed on the surface of the radar wave-absorbing layer by means of suspension supersonic spraying in combination with a shielding template, and a plurality of square through holes arranged in an array are arranged on the shielding template.
[0039] According to the embodiments of the application, forming the radar wave-absorbing layer on the surface of the corrosion-resistant layer comprises:
[0040] a first sub-wave-absorbing layer is formed on the surface of the corrosion-resistant layer by means of atmospheric plasma spraying;
[0041] a second sub-wave-absorbing layer is formed on the surface of the first sub-wave-absorbing layer by means of suspension plasma spraying.
[0042] According to the embodiments of the application, the preparation method meets at least one of the following conditions:
[0043] (1) the spraying parameters for forming the bonding layer comprise: a spraying distance of 130-180 mm, an argon flow rate of 30-40 slpm, a hydrogen flow rate of 6-10 slpm, and a power of 26-35 kW;
[0044] (2) the spraying parameters for forming the first sub-corrosion-resistant layer comprise: a spraying distance of 100-140 mm, an argon flow rate of 36-47 slpm, a hydrogen flow rate of 8-13 slpm, and a power of 32-42 kW;
[0045] (3) the spraying parameters for forming the second sub-corrosion-resistant layer include: a spraying distance of 100-140 mm, an argon flow rate of 36-47 slpm, a hydrogen flow rate of 8-13 slpm, and a power of 32-42 kW;
[0046] (4) the spraying parameters for forming the third sub-corrosion-resistant layer include: a spraying distance of 50-100 mm, an argon flow rate of 40-50 slpm, a hydrogen flow rate of 6-12 slpm, a liquid delivery flow rate of 40-80 ml / min, and a power of 45-55 kW;
[0047] (5) the spraying parameters for forming the first sub-radar-absorbing layer include: a spraying distance of 100-140 mm, an argon flow rate of 36-46 slpm, a hydrogen flow rate of 8-12 slpm, and a power of 35-42 kW;
[0048] (6) the spraying parameters for forming the second sub-radar-absorbing layer include: a spraying distance of 90-130 mm, an argon flow rate of 36-46 slpm, a hydrogen flow rate of 8-12 slpm, a power of 30-40 kW, and a liquid delivery flow rate of 40-60 ml / min;
[0049] (7) the spraying parameters for forming the infrared stealth layer include: a spraying distance of 150-250 mm, an oxygen pressure of 0.6-1.2 MPa, a hydrogen pressure of 0.4-1.4 MPa, a liquid delivery flow rate of 50-110 ml / min, and a power of 32-40 kW.
[0050] Compared with the prior art, the application has the following beneficial effects:
[0051] The corrosion-resistant layer, the radar-absorbing layer, and the infrared stealth layer of the application can cooperate with each other to enable the integrated coating of the application to simultaneously have excellent corrosion-resistant effect, excellent radar stealth effect, and excellent infrared stealth effect at an ultra-high temperature. Specifically, the integrated coating of the application has low infrared emissivity, high radar wave absorption characteristics, and excellent water vapor corrosion resistance, and can be effectively served for a long time at a temperature above 1400℃.
[0052] The integrated coating with low water-oxygen corrosion rate, high radar reflectivity, and low infrared emissivity can be prepared on the surface of a ceramic substrate by using the preparation method of the application. The integrated coating prepared by the application has excellent corrosion resistance and radar-infrared compatible stealth performance, so that the corresponding hot-end component can be safely and effectively served at an ultra-high temperature. BRIEF DESCRIPTION OF DRAWINGS
[0053] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following will briefly introduce the drawings needed to be used in the embodiments. It should be understood that the following drawings only show some of the embodiments of the present application, and therefore should not be regarded as limiting the scope of the present application.
[0054] Figure 1 A schematic diagram of the profile of the anti-corrosion and radar-infrared compatible stealth function integrated coating of the present application;
[0055] Figure 2 SEM profile of the Ti3SiC2@YSZ material used in the embodiments of the present application;
[0056] Figure 3 SEM profile of the integrated coating prepared in Embodiment 1 of the present application.
[0057] Explanation of reference signs:
[0058] 100-ceramic substrate, 200-integrated coating, 210-bonding layer, 220-anti-corrosion layer, 221-first sub-anti-corrosion layer, 222-second sub-anti-corrosion layer, 223-third sub-anti-corrosion layer, 230-radar wave absorbing layer, 231-first sub-wave absorbing layer, 232-second sub-wave absorbing layer, 240-infrared stealth layer. DETAILED DESCRIPTION
[0059] As used herein:
[0060] “Prepared from” is synonymous with “comprising”. The terms “comprising”, “including”, “having” or “with” or any other variant thereof, as used in this document, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to those elements but can include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
[0061] The conjunction “consisting of” excludes any element, step, or ingredient not specified. If used in a claim, this phrase will close the claim to the addition of any element not specified. When this phrase is used in a clause of a claim body, it only limits the clause in which it is used to exclude any element not specified; it does not exclude elements added in other clauses of the same claim.
[0062] When expressing amounts, concentrations, or other values or parameters of a range, preferably a range, or a series of upper preferred values and lower preferred values, it should be understood that the disclosure specifically encompasses all ranges formed from any pair of an upper limit or preferred value and a lower limit or preferred value, whether or not the range is expressly disclosed. For example, where a range "1-5" is disclosed, the disclosure is to be interpreted to include ranges such as "1-4," "1-3," "1-2," "1-2 and 4-5," "1-3 and 5," etc. When numerical ranges are disclosed, unless otherwise stated, the range is intended to include both the upper and lower values and all intervening values of the range, as well as the integers within the range.
[0063] In these embodiments, the parts and percentages described are by mass, unless otherwise indicated.
[0064] "Mass parts" refers to a basic unit of measurement that represents the mass ratio relationship of multiple components, 1 part can represent any unit mass, such as 1 g, 2.689 g, etc. If we say that the mass parts of component A is a parts, and the mass parts of component B is b parts, it means that the mass ratio of component A to component B is a:b. Alternatively, it means that the mass of component A is aK, and the mass of component B is bK (K is an arbitrary number, indicating a multiple factor). It should not be misunderstood that, unlike mass parts, the sum of the mass parts of all components is not limited to 100 parts.
[0065] "and / or" is used to indicate that one or both of the described conditions can occur, for example, A and / or B includes (A and B) and (A or B).
[0066] An anti-corrosion and radar-infrared compatible stealth function integrated coating, referring to Figure 1 The integrated coating 200 is arranged on the ceramic substrate 100;
[0067] The integrated coating 200 includes a bonding layer 210, an anti-corrosion layer 220, a radar wave absorbing layer 230, and an infrared stealth layer 240 arranged in layers, and the bonding layer 210 is arranged on the surface of the ceramic substrate 100;
[0068] The anti-corrosion layer 220 includes a first sub-anti-corrosion layer 221, a second sub-anti-corrosion layer 222, and a third sub-anti-corrosion layer 223 arranged in layers, and the first sub-anti-corrosion layer 221 is arranged on the surface of the bonding layer 210;
[0069] The material forming the first sub-anti-corrosion layer includes Yb2Si2O7 and a first pore-forming agent, and the mass of the first pore-forming agent accounts for 15-28% of the total mass of Yb2Si2O7 and the first pore-forming agent; the coefficient of thermal expansion (CTE) of Yb2Si2O7 material is relatively low, which is 4.0×10 -6 / K to 6.0 x 10 -6 / K, the toughness of the material is high (KIC≈2.8 MPa·m 1 / 2 ).
[0070] The material forming the second sub-corrosion-resistant layer comprises (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 and a second pore-forming agent, the mass of the second pore-forming agent accounting for 8-18% of the total mass of (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 and the second pore-forming agent;
[0071] The material forming the third sub-corrosion-resistant layer comprises (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7.
[0072] In some embodiments, the first pore-forming agent and the second pore-forming agent are both PVA.
[0073] The raw material of the second sub-corrosion-resistant layer and the third sub-corrosion-resistant layer uses a high-entropy material (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7, by introducing multi-element ions with different ionic radii—Yb 3+ (0.985 Å), Y 3+ (1.019 Å), Er 3+ (1.004 Å), Lu 3+ (0.977 Å), and Sc 3+ (0.885 Å), the lattice distortion effect can be effectively induced, the diffusion energy barrier of oxygen ions is increased by 3 times, the penetration of corrosive media is effectively blocked, and the configuration entropy ΔS mix =1.61R of the five-element equimolar solid solution is much higher than the critical value (1.5R) for forming a solid solution, ensuring the stability of the monoclinic phase.
[0074] The corrosion-resistant layer, the radar wave-absorbing layer, and the infrared stealth layer of the present application cooperate with each other, so that the integrated coating still has excellent corrosion resistance, radar-infrared compatible stealth performance at ultra-high temperature.
[0075] In some embodiments, the (Yb0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 The preparation method of Yb2Si2O7 includes:
[0076] (a) weighing each raw material according to the stoichiometric ratio of Yb2O3, Y2O3, Er2O3, Lu2O3, Sc2O3 and SiO2 as raw materials; 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 Sc
[0077] (b) putting the weighed raw materials in step (a) and zirconia balls and water together in a ball mill jar, and performing ball milling mixing, the ball milling time being 24-48 h, to obtain a uniformly mixed slurry;
[0078] (c) drying the slurry obtained in step (b), the drying temperature being 130-160℃, and the drying time being 12-18 h, to obtain a mixed powder, and then performing a pre-sintering reaction on the mixed powder in an air atmosphere, the pre-sintering reaction temperature being 1000-1300℃, and the pre-sintering reaction time being 4-10 h, to obtain a pre-sintered powder;
[0079] (d) mixing the pre-sintered powder obtained in step (c) and water, and performing secondary ball milling, the ball milling time being 24-48 h, to obtain a uniformly mixed slurry;
[0080] (e) drying the slurry obtained in step (d), the drying temperature being 130-160℃, and the drying time being 12-18 h, and then performing a sintering reaction in an air atmosphere, the sintering reaction temperature being 1300-1600℃, and the sintering reaction time being 8-20 h, to obtain a (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 Sc
[0081] According to the embodiments of the present application, the corrosion-resistant layer satisfies at least one of the following conditions:
[0082] (1) the thickness of the corrosion-resistant layer is 100-250 μm;
[0083] For example, the thickness of the corrosion-resistant layer is 100 μm, 150 μm, 200 μm, 250 μm, or any value between 100 μm and 250 μm.
[0084] (2) the thickness of the first sub-anticorrosion layer is 40-100 μm, the thickness of the second sub-anticorrosion layer is 40-100 μm, and the thickness of the third sub-anticorrosion layer is 20-50 μm;
[0085] The first sub-anticorrosion layer with a larger thickness can match the thermal expansion coefficient, the second sub-anticorrosion layer with a larger thickness can inhibit crack propagation, and the third sub-anticorrosion layer with a smaller thickness can inhibit the downward corrosion of corrosion media including CMAS and water oxygen, thereby playing an excellent anticorrosion effect.
[0086] For example, the thickness of the first sub-anticorrosion layer is 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, or any value between 40-100 μm.
[0087] The thickness of the second sub-anticorrosion layer is 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, or any value between 40-100 μm.
[0088] The thickness of the third sub-anticorrosion layer is 20 μm, 30 μm, 40 μm, 50 μm, or any value between 20-50 μm.
[0089] (3) the porosity of the first sub-anticorrosion layer is greater than the porosity of the second sub-anticorrosion layer, and the porosity of the second sub-anticorrosion layer is greater than the porosity of the third sub-anticorrosion layer;
[0090] The first sub-anticorrosion layer and the second sub-anticorrosion layer have a larger porosity, which can effectively inhibit crack propagation. Moreover, the porosity of the first sub-anticorrosion layer, the second sub-anticorrosion layer, and the third sub-anticorrosion layer of the present application gradually decreases, and the gradient transition of the porosity can ensure the bonding performance of the third sub-anticorrosion layer.
[0091] The second sub-anticorrosion layer and the third sub-anticorrosion layer are prepared by different processes. In the preparation of the second sub-anticorrosion layer, a pore-forming agent is added to the raw material, and the second sub-anticorrosion layer with a porous structure can be prepared by atmospheric plasma spraying, which can effectively reduce the coating stress. The third sub-anticorrosion layer prepared by suspension plasma spraying has a dense structure, which can play an excellent anticorrosion effect.
[0092] (4) the porosity of the first sub-anticorrosion layer is 20-30%, and the porosity of the second sub-anticorrosion layer is 15-25%.
[0093] The first sub-anticorrosion layer and the second sub-anticorrosion layer can inhibit crack propagation through the porous structure, wherein the first sub-anticorrosion layer in the lower layer has a higher porosity, the second sub-anticorrosion layer in the middle layer has a relatively lower porosity, and the bonding performance of the third sub-anticorrosion layer in the upper layer can be ensured through the gradient transition of the porosity.
[0094] For example, the porosity of the first sub-erosion-resistant layer is 20%, 25%, 30%, or any value between 20-30%, and the porosity of the second sub-erosion-resistant layer is 15%, 20%, 25%, or any value between 15-25%.
[0095] According to an embodiment of the present application, the adhesive layer satisfies at least one of the following conditions:
[0096] (1) the material forming the adhesive layer comprises Si;
[0097] (2) the thickness of the adhesive layer is 60-110 μm.
[0098] For example, the thickness of the adhesive layer is 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, 110 μm, or any value between 60-110 μm.
[0099] According to an embodiment of the present application, the radar wave absorbing layer satisfies at least one of the following conditions:
[0100] (1) the radar wave absorbing layer comprises a first sub-wave absorbing layer 231 and a second sub-wave absorbing layer 232 arranged in layers, the first sub-wave absorbing layer 231 is arranged on the surface of the erosion-resistant layer 220, the material forming the first sub-wave absorbing layer comprises La 0.7 Sr 0.3 MnO3, Al2O3 and SiO2, and the material forming the second sub-wave absorbing layer comprises Ti3SiC2@YSZ and Al2O3;
[0101] La 0.7 Sr 0.3 MnO3 has low-frequency wave absorbing properties, by introducing Al2O3 with low dielectric constant, the impedance matching of the coating can be optimized, and the low-frequency wave absorbing function of the coating can be realized; by introducing SiO2 with low CTE and melting point, the CTE of the first sub-wave absorbing layer can be reduced to realize the transition of the radar wave absorbing layer and the erosion-resistant layer, and improve the thermal stability of the coating.
[0102] The second sub-wave-absorbing layer can serve as a medium-high frequency wave-absorbing layer. Ti3SiC2 has excellent high-temperature wave-absorbing performance. However, Ti3SiC2 material will be oxidized and phase-changed when it is sprayed by conventional atmospheric plasma, which will reduce the wave-absorbing capacity. In one aspect, the Ti3SiC2 is coated with YSZ to prepare Ti3SiC2@YSZ, which can improve the oxidation resistance of Ti3SiC2 during spraying and service. In another aspect, the suspension plasma spraying method with low pyrolysis and low phase change is used to further ensure the phase structure stability of Ti3SiC2 during coating preparation. In addition, the high electrical conductivity of Ti3SiC2 will cause strong reflection of electromagnetic waves on the surface of the coating, thereby reducing the wave-absorbing performance of the coating. Therefore, by adding Al2O3 with low dielectric constant for impedance matching and optimization of the coating, the excellent wave-absorbing performance of the coating can be achieved.
[0103] The Ti3SiC2@YSZ material comprises Ti3SiC2 and a YSZ layer coated on the outer surface of the Ti3SiC2. The YSZ layer can completely coat the Ti3SiC2, which can improve the oxidation resistance of Ti3SiC2 while reducing the influence on the wave-absorbing performance of Ti3SiC2.
[0104] The preparation method of Ti3SiC2@YSZ comprises the following steps:
[0105] (a) Ti3SiC2 powder and 8YSZ powder are weighed in a mass ratio of 9:1-7:3, and are placed in a ball mill tank together with zirconia balls. Polyvinyl alcohol is added as a binder, and the mass of polyvinyl alcohol accounts for 3-6% of the total mass of Ti3SiC2 powder and 8YSZ powder. Deionized water is used as a medium, and ball milling is performed for 24-48 hours to obtain a uniformly mixed slurry;
[0106] (b) The slurry obtained in (a) is spray dried. The rotation speed of the spray head is 25-35 r / s, the inlet temperature is 250-350 DEG C, and the outlet temperature is 110-130 DEG C. Ti3SiC2 mixed with 8YSZ spherical powder is obtained;
[0107] (c) The Ti3SiC2 mixed with 8YSZ spherical powder and 8YSZ powder are weighed in a mass ratio of 3:1-2:1, and are placed in a ball mill tank. Polyvinyl alcohol is added as a binder, and the mass of polyvinyl alcohol accounts for 5-10% of the total mass of Ti3SiC2 mixed with 8YSZ spherical powder and 8YSZ powder. Water is used as a medium, no grinding balls are added, and the mixture is mixed in a ball mill for 10-30 minutes to obtain a uniformly mixed slurry;
[0108] (d) The slurry obtained in (c) is spray dried. The rotation speed of the spray head is 15-30 r / s, the inlet temperature is 250-350 DEG C, and the outlet temperature is 110-130 DEG C. Ti3SiC2@YSZ material is obtained.
[0109] (2) the thickness of the radar wave absorbing layer is 700-800 μm.
[0110] For example, the thickness of the radar wave absorbing layer is 700 μm, 750 μm, 800 μm, or any value between 700-800 μm.
[0111] According to an embodiment of the present application, the radar wave absorbing layer satisfies at least one of the following conditions:
[0112] (1) the thickness ratio of the first sub-wave absorbing layer to the second sub-wave absorbing layer is 5:4-7:3;
[0113] For example, the thickness ratio of the first sub-wave absorbing layer to the second sub-wave absorbing layer is 5:4, 6:4, 7:4, 5:3, 6:3, 7:3, or any value between 5:4-7:3.
[0114] The first sub-wave absorbing layer with a larger thickness can realize the CTE transition of the corrosion-resistant layer to the wave absorbing layer, ensuring the overall bonding performance of the coating.
[0115] (2) in the material forming the first sub-wave absorbing layer, the mass ratio of La 0.7 Sr 0.3 MnO3 to Al2O3 and SiO2 is (1-3):(2-4):5;
[0116] For example, the mass ratio of La 0.7 Sr 0.3 MnO3 to Al2O3 and SiO2 is 1:2:5, 2:2:5, 3:2:5, 1:3:5, 2:3:5, 3:3:5, 1:4:5, 2:4:5, 3:4:5, or any value between (1-3):(2-4):5;
[0117] (3) in the material forming the second sub-wave absorbing layer, the mass of Ti3SiC2@YSZ accounts for (45-65)% of the mass of the material forming the second sub-wave absorbing layer.
[0118] For example, the mass of Ti3SiC2@YSZ accounts for 45%, 50%, 55%, 60%, 65%, or any value between (45-65)% of the mass of the material forming the second sub-wave absorbing layer.
[0119] According to an embodiment of the present application, the area of the orthographic projection of the infrared stealth layer on the radar wave absorbing layer is less than the area of the radar wave absorbing layer, and the orthographic projection of the infrared stealth layer on the radar wave absorbing layer is a plurality of array-arranged squares.
[0120] The side length of the square is 0.8-3.5 mm, and the interval distance between adjacent squares is 0.5-1.2 times the side length of the square.
[0121] For example, the square has a side length of 0.8 mm, 1 mm, 1.5 mm, 2 mm, 2.5 mm, 3 mm, 3.5 mm, or any value between 0.8-3.5 mm, and the interval distance between adjacent squares is 0.5 times, 1 times, 1.2 times, or any value between 0.5-1.2 times of the side length of the square.
[0122] The periodic structure of the infrared stealth layer is beneficial to improving the overall wave absorption performance of the coating.
[0123] According to the embodiments of the present application, the infrared stealth layer satisfies at least one of the following conditions:
[0124] (1) The material forming the infrared stealth layer comprises Ti3SiC2 and a noble metal material, the noble metal material comprises at least one of AgPd, Pt, and Pd, and the mass of the noble metal material accounts for 60-80% of the mass of the material forming the infrared stealth layer;
[0125] For example, the mass of the noble metal material accounts for 60%, 70%, 80%, or any value between 60-80% of the mass of the material forming the infrared stealth layer;
[0126] The infrared stealth layer of the present application uses MAX ceramic and noble metal material as coating material, the addition of Ti3SiC2 can enhance the hardness, wear resistance, high temperature resistance, etc. of the coating, in addition, Ti3SiC2 can also play a certain wave absorption performance; a dense metasurface layer of Ti3SiC2 reinforced noble metal with periodic structure is prepared by using the suspension supersonic spraying method, and the noble metal material with low emissivity can make the coating have excellent low infrared emissivity, i.e. infrared stealth characteristics.
[0127] The noble metal material has extremely low infrared emissivity, and the mass of the noble metal material of the present application accounts for 60-80% of the mass of the material forming the infrared stealth layer, and a higher content of noble metal material can ensure the overall low infrared emissivity characteristics of the coating, and the addition of 20-40% Ti3SiC2 can ensure the high temperature stability of the coating.
[0128] (2) The thickness of the infrared stealth layer is 20-50 μm.
[0129] For example, the thickness of the infrared stealth layer is 20 μm, 30 μm, 40 μm, 50 μm, or any value between 20-50 μm.
[0130] The present application also provides a preparation method of the corrosion-resistant and radar-infrared compatible stealth function integrated coating as described above, comprising:
[0131] The bonding layer is formed on the surface of the ceramic substrate by atmospheric plasma spraying;
[0132] The first sub-corrosion-resistant layer, the second sub-corrosion-resistant layer and the third sub-corrosion-resistant layer are formed on the surface of the bonding layer by atmospheric plasma spraying, the second sub-corrosion-resistant layer is formed on the surface of the first sub-corrosion-resistant layer by suspension plasma spraying, and the third sub-corrosion-resistant layer is formed on the surface of the second sub-corrosion-resistant layer by suspension plasma spraying, so as to form the corrosion-resistant layer.
[0133] The radar wave-absorbing layer is formed on the surface of the corrosion-resistant layer.
[0134] The infrared stealth layer is formed on the surface of the radar wave-absorbing layer by suspension supersonic spraying in combination with the shielding template, and the shielding template is provided with a plurality of square through holes arranged in an array.
[0135] In some embodiments, the preparation of the infrared stealth layer comprises: covering the shielding template on the surface of the radar wave-absorbing layer; and forming the infrared stealth layer on the surface of the radar wave-absorbing layer through the square through holes of the shielding template by suspension supersonic spraying, so that the shape of the infrared stealth layer is a plurality of square shapes arranged in an array.
[0136] According to the embodiments of the present application, the radar wave-absorbing layer is formed on the surface of the corrosion-resistant layer, which comprises:
[0137] The first sub-wave-absorbing layer is formed on the surface of the corrosion-resistant layer by atmospheric plasma spraying.
[0138] The second sub-wave-absorbing layer is formed on the surface of the first sub-wave-absorbing layer by suspension plasma spraying.
[0139] According to the embodiments of the present application, the preparation method satisfies at least one of the following conditions:
[0140] (1) The spraying parameters for forming the bonding layer comprise: a spraying distance of 130 mm-180 mm, an argon flow rate of 30-40 slpm, a hydrogen flow rate of 6-10 slpm, and a power of 26-35 kW;
[0141] For example, the spraying parameters for forming the bonding layer comprise: a spraying distance of 130 mm, 150 mm, 180 mm or any value between 130 mm and 180 mm, an argon flow rate of 30 slpm, 35 slpm, 40 slpm or any value between 30 slpm and 40 slpm, a hydrogen flow rate of 6 slpm, 8 slpm, 10 slpm or any value between 6 slpm and 10 slpm, and a power of 26 kW, 30 kW, 35 kW or any value between 26 kW and 35 kW.
[0142] (2) the spraying parameters for forming the first sub-corrosion-resistant layer include: a spraying distance of 100-140 mm, an argon flow rate of 36-47 slpm, a hydrogen flow rate of 8-13 slpm, and a power of 32-42 kW;
[0143] For example, the spraying parameters for forming the first sub-corrosion-resistant layer include: a spraying distance of 100 mm, 120 mm, 140 mm, or any value between 100 mm and 140 mm, an argon flow rate of 36 slpm, 42 slpm, 47 slpm, or any value between 36 slpm and 47 slpm, a hydrogen flow rate of 8 slpm, 10 slpm, 13 slpm, or any value between 8 slpm and 13 slpm, and a power of 32 kW, 35 kW, 42 kW, or any value between 32 kW and 42 kW.
[0144] (3) the spraying parameters for forming the second sub-corrosion-resistant layer include: a spraying distance of 100-140 mm, an argon flow rate of 36-47 slpm, a hydrogen flow rate of 8-13 slpm, and a power of 32-42 kW;
[0145] For example, the spraying parameters for forming the second sub-corrosion-resistant layer include: a spraying distance of 100 mm, 120 mm, 140 mm, or any value between 100 mm and 140 mm, an argon flow rate of 36 slpm, 42 slpm, 47 slpm, or any value between 36 slpm and 47 slpm, a hydrogen flow rate of 8 slpm, 10 slpm, 13 slpm, or any value between 8 slpm and 13 slpm, and a power of 32 kW, 35 kW, 42 kW, or any value between 32 kW and 42 kW.
[0146] (4) the spraying parameters for forming the third sub-corrosion-resistant layer include: a spraying distance of 50-100 mm, an argon flow rate of 40-50 slpm, a hydrogen flow rate of 6-12 slpm, a liquid delivery flow rate of 40-80 ml / min, and a power of 45-55 kW;
[0147] For example, the spraying parameters for forming the third sub-corrosion-resistant layer include: a spraying distance of 50 mm, 80 mm, 100 mm, or any value between 50 mm and 100 mm, an argon flow rate of 40 slpm, 45 slpm, 50 slpm, or any value between 40 slpm and 50 slpm, a hydrogen flow rate of 6 slpm, 10 slpm, 12 slpm, or any value between 6 slpm and 12 slpm, a liquid delivery flow rate of 40 ml / min, 50 ml / min, 60 ml / min, 70 ml / min, 80 ml / min, or any value between 40 ml / min and 80 ml / min, and a power of 45 kW, 50 kW, 55 kW, or any value between 45 kW and 55 kW.
[0148] In some embodiments, the raw material for preparing the third anti-corrosion layer is (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 suspension.
[0149] The method for preparing (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 suspension includes:
[0150] (a) mixing (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 powder, a dispersant and a solvent to obtain a mixed system, the dispersant is at least one of polyacrylammonium, polyethyleneimine and gum arabic, the solvent is at least one of deionized water, anhydrous ethanol, isopropanol and acetone, and the mass ratio of (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 powder, the dispersant and the solvent is 50:(2-4):(75-79);
[0151] (b) placing the mixed system obtained in step (a) and zirconia balls in a ball mill tank together, and performing ball milling, the ball milling time is 8-30 h;
[0152] (c) performing ultrasonic treatment on the suspension after ball milling, the ultrasonic power is 300-800 W, and the ultrasonic time is 10-50 min, to obtain (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 suspension.
[0153] (5) the spraying parameters for forming the first sub-wave-absorbing layer include: the spraying distance is 100 mm-140 mm, the argon flow rate is 36-46 slpm, the hydrogen flow rate is 8-12 slpm, and the power is 35-42 kW;
[0154] For example, the spraying parameters for forming the first sub-wave-absorbing layer include: a spraying distance of 100 mm, 120 mm, 140 mm, or any value between 100 mm and 140 mm, an argon flow rate of 36 slpm, 42 slpm, 46 slpm, or any value between 36 slpm and 46 slpm, a hydrogen flow rate of 8 slpm, 10 slpm, 12 slpm, or any value between 8 slpm and 12 slpm, and a power of 35 kW, 38 kW, 42 kW, or any value between 35 kW and 42 kW.
[0155] (6) The spraying parameters for forming the second sub-wave-absorbing layer include: a spraying distance of 90 mm to 130 mm, an argon flow rate of 36 slpm to 46 slpm, a hydrogen flow rate of 8 slpm to 12 slpm, a power of 30 kW to 40 kW, and a liquid delivery flow rate of 40 ml / min to 60 ml / min.
[0156] For example, the spraying parameters for forming the second sub-wave-absorbing layer include: a spraying distance of 90 mm, 110 mm, 130 mm, or any value between 90 mm and 130 mm, an argon flow rate of 36 slpm, 42 slpm, 46 slpm, or any value between 36 slpm and 46 slpm, a hydrogen flow rate of 8 slpm, 10 slpm, 12 slpm, or any value between 8 slpm and 12 slpm, a power of 30 kW, 35 kW, 40 kW, or any value between 30 kW and 40 kW, and a liquid delivery flow rate of 40 ml / min, 50 ml / min, 60 ml / min, or any value between 40 ml / min and 60 ml / min.
[0157] In some embodiments, the raw material for preparing the second sub-wave-absorbing layer is a suspension containing Ti3SiC2@YSZ and Al2O3.
[0158] The method for preparing the suspension containing Ti3SiC2@YSZ and Al2O3 includes:
[0159] (a) mixing Ti3SiC2@YSZ, Al2O3, a dispersant, and a solvent to obtain a mixed system, the dispersant being at least one of polyammonium acrylate, polyethyleneimine, and gum arabic, the solvent being at least one of deionized water, anhydrous ethanol, isopropanol, and acetone, and the mass ratio of Ti3SiC2@YSZ to Al2O3, the dispersant, and the solvent being 25: (23-27): (2-4): (75-79);
[0160] (b) placing the mixed system obtained in step (a) in a ball mill jar and performing dispersion mixing for 8-30 h;
[0161] (c) the suspension after ball milling is subjected to ultrasonic treatment, the ultrasonic power is 300-800 W, and the ultrasonic time is 10-50 min, to obtain a suspension containing Ti3SiC2@YSZ and Al2O3.
[0162] (7) The spraying parameters for forming the infrared stealth layer include: a spraying distance of 150-250 mm, an oxygen pressure of 0.6-1.2 MPa, a hydrogen pressure of 0.4-1.4 MPa, a liquid flow rate of 50-110 ml / min, and a power of 32-40 kW.
[0163] For example, the spraying parameters for forming the infrared stealth layer include: a spraying distance of 150 mm, 200 mm, 250 mm, or any value between 150 mm and 250 mm, an oxygen pressure of 0.6 MPa, 0.9 MPa, 1.2 MPa, or any value between 0.6 MPa and 1.2 MPa, a hydrogen pressure of 0.4 MPa, 0.9 MPa, 1.4 MPa, or any value between 0.4 MPa and 1.4 MPa, a liquid flow rate of 50 ml / min, 60 ml / min, 70 ml / min, 80 ml / min, 90 ml / min, 100 ml / min, 110 ml / min, or any value between 50 ml / min and 110 ml / min, and a power of 32 kW, 36 kW, 40 kW, or any value between 32 kW and 40 kW.
[0164] In some embodiments, the raw material for preparing the infrared stealth layer is a suspension containing Ti3SiC2 and Pt.
[0165] The method for preparing the suspension containing Ti3SiC2 and Pt includes:
[0166] (a) mixing Ti3SiC2, Pt, a dispersant, and a solvent to obtain a mixed system, the dispersant being at least one of polyammonium acrylate, polyethyleneimine, and gum arabic, the solvent being at least one of deionized water, anhydrous ethanol, isopropyl alcohol, and acetone, and the mass ratio of Ti3SiC2 to Pt, the dispersant, and the solvent being 10:(38-42):(2-4):(75-79);
[0167] (b) placing the mixed system obtained in step (a) and zirconia balls in a ball milling tank together for ball milling, and the ball milling time is 8-30 h;
[0168] (c) subjecting the suspension after ball milling to ultrasonic treatment, the ultrasonic power being 300-800 W, and the ultrasonic time being 10-50 min, to obtain a suspension containing Ti3SiC2 and Pt.
[0169] The embodiments of the present application will be described in detail below with specific examples, but those skilled in the art will understand that the following examples are only for illustration of the present application and should not be regarded as limiting the scope of the present application. The specific conditions are not specified in the examples, and the conventional conditions or the conditions recommended by the manufacturer are used. The reagents or instruments used are not specified by the manufacturer, and are conventional products that can be obtained by commercial purchase.
[0170] The raw material information used in the examples and comparative examples of the present application is as follows:
[0171] Ti3SiC2@YSZ is prepared by the following method:
[0172] (a) Ti3SiC2 powder and 8YSZ powder are weighed in a mass ratio of 9:1, and zirconia balls are placed together in a ball mill tank, polyvinyl alcohol is added as a binder, the mass of polyvinyl alcohol accounts for 3% of the total mass of Ti3SiC2 powder and 8YSZ powder, deionized water is used as a medium, and ball milling is performed for 36 h to obtain a uniformly mixed slurry;
[0173] (b) The slurry obtained in (a) is spray dried, the spray head rotation speed is 35 r / s, the inlet temperature is 350°C, and the outlet temperature is 130°C to obtain Ti3SiC2 mixed 8YSZ spherical powder;
[0174] (c) The Ti3SiC2 mixed 8YSZ spherical powder and 8YSZ powder are weighed in a mass ratio of 2:1 and placed in a ball mill tank, polyvinyl alcohol is added as a binder, the mass of polyvinyl alcohol accounts for 6% of the total mass of Ti3SiC2 mixed 8YSZ spherical powder and 8YSZ powder, deionized water is used as a medium, no grinding balls are added, and the mixture is mixed in a ball mill for 10 min to obtain a uniformly mixed slurry;
[0175] (d) The slurry obtained in (c) is spray dried, the spray head rotation speed is 30 r / s, the inlet temperature is 350°C, and the outlet temperature is 110°C to obtain Ti3SiC2@YSZ material, the SEM cross-sectional view of Ti3SiC2@YSZ material is shown in Figure 2 It can be seen from Figure 2 that the Ti3SiC2@YSZ material has a core-shell structure.
[0176] Example 1
[0177] Example 1 provides an anti-corrosion and radar-infrared compatible stealth function integrated coating, and the preparation method comprises:
[0178] (1) preparing a bonding layer on a SiC / SiC f ceramic substrate;
[0179] Si is used as raw material, and a bonding layer is formed on the surface of a ceramic substrate by atmospheric plasma spraying;
[0180] The spraying parameters for forming the bonding layer include a spraying distance of 135 mm, an argon flow rate of 40 slpm, a hydrogen flow rate of 8 slpm, and a power of 32 kW;
[0181] The thickness of the bonding layer is 80 μm.
[0182] (2) An anti-corrosion layer is formed on the surface of the bonding layer;
[0183] (2-1) A first sub-anti-corrosion layer is prepared on the bonding layer;
[0184] Yb2Si2O7 and PVA are used as raw materials, the mass of PVA accounts for 25% of the total mass of Yb2Si2O7 and PVA, and the first sub-anti-corrosion layer is formed on the surface of the bonding layer by atmospheric plasma spraying;
[0185] The spraying parameters for forming the first sub-anti-corrosion layer include a spraying distance of 120 mm, an argon flow rate of 39 slpm, a hydrogen flow rate of 12 slpm, and a power of 42 kW;
[0186] (2-2) A second sub-anti-corrosion layer is prepared on the first sub-anti-corrosion layer;
[0187] (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 and PVA are used as raw materials, the mass of PVA accounts for 15% of the total mass of (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 and PVA, and the second sub-anti-corrosion layer is formed on the surface of the first sub-anti-corrosion layer by atmospheric plasma spraying;
[0188] The spraying parameters for forming the second sub-anti-corrosion layer include a spraying distance of 120 mm, an argon flow rate of 40 slpm, a hydrogen flow rate of 13 slpm, and a power of 42 kW;
[0189] (2-3) A third sub-anti-corrosion layer is prepared on the second sub-anti-corrosion layer;
[0190] (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2A third sub-corrosion-resistant layer is formed on the surface of the second sub-corrosion-resistant layer by using suspension plasma spraying with (Yb
[0191] (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 powder preparation method comprises:
[0192] (a) Yb2O3, Y2O3, Er2O3, Lu2O3, Sc2O3 and SiO2 as raw materials, according to (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 stoichiometric ratio of each raw material is weighed;
[0193] (b) the raw materials weighed in step (a) and zirconia balls, deionized water are put into a ball mill pot together, and ball milling is carried out, the ball milling time is 48h, and a uniformly mixed slurry is obtained;
[0194] (c) the slurry obtained in step (b) is dried, the drying temperature is 160℃, the drying time is 12h, a mixed powder is obtained, and then the mixed powder is subjected to a pre-sintering reaction in an air atmosphere, the pre-sintering reaction temperature is 1200℃, and the pre-sintering reaction time is 6h, to obtain a pre-sintered powder;
[0195] (d) the pre-sintered powder obtained in step (c) and deionized water are mixed, and secondary ball milling is carried out, the ball milling time is 24h, and a uniformly mixed slurry is obtained;
[0196] (e) the slurry obtained in step (d) is dried, the drying temperature is 160℃, the drying time is 12h, and then a sintering reaction is carried out in an air atmosphere, the sintering reaction temperature is 1400℃, and the sintering reaction time is 12h, to obtain (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 powder.
[0197] The method for preparing (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 suspension comprises:
[0198] (a) (Yb 0.2 Y 0.2 Er 0.2Lu 0.2 Sc 0.2 )2Si2O7 powder, a dispersant and a solvent are mixed to obtain a mixed system, the dispersant is ammonium polyacrylate, and the solvent is deionized water, (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 The mass ratio of (Yb
[0199] (b) the mixed system obtained in step (a) and zirconium oxide balls are placed in a ball mill tank together, and ball milling is performed for 24 h;
[0200] (c) the suspension after ball milling is subjected to ultrasonic treatment, the ultrasonic power is 600 W, and the ultrasonic time is 20 min, to obtain a (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 suspension.
[0201] The spraying parameters for forming the third sub-anti-corrosion layer include: a spraying distance of 70 mm, an argon flow rate of 45 slpm, a hydrogen flow rate of 12 slpm, a power of 50 kW, and a liquid feeding flow rate of 45 ml / min;
[0202] The thickness of the first sub-anti-corrosion layer is 60 μm, the thickness of the second sub-anti-corrosion layer is 40 μm, and the thickness of the third sub-anti-corrosion layer is 25 μm; the thickness of the anti-corrosion layer is 125 μm; the porosity of the first sub-anti-corrosion layer is 28%, and the porosity of the second sub-anti-corrosion layer is 23%.
[0203] (3) forming a radar wave-absorbing layer on the surface of the anti-corrosion layer;
[0204] (3-1) preparing a first sub-wave-absorbing layer on the third sub-anti-corrosion layer;
[0205] La 0.7 Sr 0.3 MnO3, Al2O3 and SiO2 are used as raw materials, wherein the mass ratio of La 0.7 Sr 0.3 MnO3 to Al2O3 and SiO2 is 3:2:5; and the first sub-wave-absorbing layer is formed on the surface of the anti-corrosion layer by using an atmospheric plasma spraying method;
[0206] The spraying parameters for forming the first sub-wave-absorbing layer include: a spraying distance of 120 mm, an argon flow rate of 40 slpm, a hydrogen flow rate of 10 slpm, and a power of 38 kW;
[0207] (3-2) preparing a second sub-wave-absorbing layer on the first sub-wave-absorbing layer;
[0208] The suspension containing Ti3SiC2@YSZ and Al2O3 is used as raw material, wherein the mass of Ti3SiC2@YSZ accounts for 50% of the total mass of Ti3SiC2@YSZ and Al2O3. The suspension plasma spraying method is used to form the second sub-wave-absorbing layer on the surface of the first sub-wave-absorbing layer;
[0209] The preparation of the suspension containing Ti3SiC2@YSZ and Al2O3 includes:
[0210] (a) mixing Ti3SiC2@YSZ, Al2O3, a dispersing agent and a solvent, the dispersing agent is polyacrylammonium, the solvent is deionized water, and the mass ratio of Ti3SiC2@YSZ powder, Al2O3 powder, dispersing agent and deionized water is 25:25:3:77;
[0211] (b) placing the mixed system obtained in step (a) in a ball mill jar for dispersion mixing, and the time is 24h;
[0212] (c) ultrasonic treatment is performed on the suspension after dispersion mixing, the ultrasonic power is 300W, and the ultrasonic time is 15min, to obtain the suspension containing Ti3SiC2@YSZ and Al2O3.
[0213] The spraying parameters for forming the second sub-wave-absorbing layer include: a spraying distance of 100mm, an argon flow rate of 42slpm, a hydrogen flow rate of 11slpm, a power of 39kW, and a liquid feeding flow rate of 50ml / min;
[0214] The thickness of the radar wave-absorbing layer is 800μm, and the thickness ratio of the first sub-wave-absorbing layer to the second sub-wave-absorbing layer is 5:3;
[0215] (4) preparing an infrared stealth layer on the radar wave-absorbing layer;
[0216] A shielding template is provided, and the shielding template is provided with a plurality of square through holes arranged in an array;
[0217] The shielding template is covered on the surface of the second sub-wave-absorbing layer;
[0218] The suspension containing Ti3SiC2 and Pt is used as raw material, and the infrared stealth layer is formed on the surface of the second sub-wave-absorbing layer through the square through holes of the shielding template, so that the shape of the infrared stealth layer is a plurality of square through holes arranged in an array.
[0219] The preparation of the suspension containing Ti3SiC2 and Pt includes:
[0220] (a) mixing Ti3SiC2, Pt, dispersant and solvent, the dispersant is ammonium polyacrylate, the solvent is deionized water, the mass ratio of Ti3SiC2: Pt: dispersant: solvent is 10:40:3:77;
[0221] (b) putting the mixed system obtained in step (a) and zirconium oxide balls into a ball mill tank together, and performing ball milling, the ball milling time is 24 h;
[0222] (c) performing ultrasonic treatment on the suspension after ball milling, the ultrasonic power is 800 W, and the ultrasonic time is 45 min, to obtain a suspension containing Ti3SiC2 and Pt.
[0223] The spraying parameters for forming the infrared stealth layer include: a spraying distance of 160 mm, an oxygen pressure of 0.8 MPa, a hydrogen pressure of 0.6 MPa, a power of 34 kW, and a liquid feeding flow rate of 60 ml / min.
[0224] The thickness of the infrared stealth layer is 30 μm.
[0225] The orthographic projection area of the infrared stealth layer on the radar wave absorbing layer is less than the area of the radar wave absorbing layer, the orthographic projection of the infrared stealth layer on the radar wave absorbing layer is a plurality of array-arranged squares, the side length of the square is 2.0 mm, and the interval distance between adjacent squares is 0.6 times the side length of the square.
[0226] The SEM cross-sectional view of the integrated coating prepared in Example 1 is shown in Figure 3 .
[0227] Example 2
[0228] The anti-corrosion and radar-infrared compatible stealth function integrated coating is prepared by referring to the method of Example 1, and the other steps and parameters are the same as those of Example 1, and the difference between Example 2 and Example 1 is that the mass of PVA in the raw material for preparing the second sub-anti-corrosion layer accounts for 9% of the total mass of (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7+PVA.
[0229] The porosity of the second sub-anti-corrosion layer in Example 2 is 15%.
[0230] Example 3
[0231] The corrosion-resistant and radar-infrared compatible stealth function integrated coating was prepared according to the method of Example 1, and other steps and parameters were the same as those of Example 1. The difference between Example 3 and Example 1 was that in the suspension containing Ti3SiC2@YSZ and Al2O3 for preparing the second sub-wave absorbing layer, the mass of Ti3SiC2@YSZ accounted for 65% of the total mass of Ti3SiC2@YSZ and Al2O3.
[0232] Example 4
[0233] The corrosion-resistant and radar-infrared compatible stealth function integrated coating was prepared according to the method of Example 1, and other steps and parameters were the same as those of Example 1. The difference between Example 4 and Example 1 was that in the suspension containing Ti3SiC2 and Pt for preparing the infrared stealth layer, the mass of Pt accounted for 60% of the total mass of Ti3SiC2 and Pt.
[0234] Comparative Example 1
[0235] The corrosion-resistant and radar-infrared compatible stealth function integrated coating was prepared according to the method of Example 1, and other steps and parameters were the same as those of Example 1. The difference between Comparative Example 1 and Example 1 was that Comparative Example 1 omitted the step of preparing the third sub-corrosion-resistant layer.
[0236] Comparative Example 2
[0237] The corrosion-resistant and radar-infrared compatible stealth function integrated coating was prepared according to the method of Example 1, and other steps and parameters were the same as those of Example 1. The difference between Comparative Example 2 and Example 1 was that in the suspension containing Ti3SiC2@YSZ and Al2O3 for preparing the second sub-wave absorbing layer, the same mass of Ti3SiC2 material was used instead of Ti3SiC2@YSZ material.
[0238] Comparative Example 3
[0239] The corrosion-resistant and radar-infrared compatible stealth function integrated coating was prepared according to the method of Example 1, and other steps and parameters were the same as those of Example 1. The difference between Comparative Example 3 and Example 1 was that in the suspension for preparing the infrared stealth layer, Pt was not added, only Ti3SiC2 was added, and the mass of Ti3SiC2 in Comparative Example 3 was equal to the total mass of Ti3SiC2 and Pt in Example 1.
[0240] Comparative Example 4
[0241] The corrosion-resistant and radar-infrared compatible stealth function integrated coating was prepared according to the method of Example 1, and other steps and parameters were the same as those of Example 1. The difference between Comparative Example 4 and Example 1 was that Comparative Example 4 omitted the step of preparing the infrared stealth layer.
[0242] Examples 1-4 and Comparative Examples 1-4 were subjected to performance tests under the same conditions, and the test methods included:
[0243] (1) Water-oxygen corrosion resistance test: performed at a temperature of 1400°C in an atmosphere of 90% H2O + 10% O2;
[0244] (2) Radar reflectivity test: tested for reflectivity in the 8-18 GHz band using the bowtie method;
[0245] (3) Infrared emissivity test: measured for emissivity in the 3-5 μm band using the energy comparison method.
[0246] The performance test results for Examples 1-4 and Comparative Examples 1-4 were as follows:
[0247] Example 1: No peeling of the coating after water-oxygen corrosion for 300 h, minimum reflectivity of -24.8 dB in the 8-18 GHz band, and infrared emissivity of 0.18 in the 3-5 μm band.
[0248] Example 2: No peeling of the coating after water-oxygen corrosion for 263 h, minimum reflectivity of -24.8 dB in the 8-18 GHz band, and infrared emissivity of 0.18 in the 3-5 μm band.
[0249] Example 3: No peeling of the coating after water-oxygen corrosion for 300 h, minimum reflectivity of -19.3 dB in the 8-18 GHz band, and infrared emissivity of 0.18 in the 3-5 μm band.
[0250] Example 4: No peeling of the coating after water-oxygen corrosion for 300 h, minimum reflectivity of -24.8 dB in the 8-18 GHz band, and infrared emissivity of 0.25 in the 3-5 μm band.
[0251] Comparative Example 1: Peeling of the coating after water-oxygen corrosion for 123 h, minimum reflectivity of -24.8 dB in the 8-18 GHz band, and infrared emissivity of 0.18 in the 3-5 μm band.
[0252] Comparative Example 2: No peeling of the coating after water-oxygen corrosion for 300 h, minimum reflectivity of -6.4 dB in the 8-18 GHz band, and infrared emissivity of 0.18 in the 3-5 μm band.
[0253] Comparative Example 3: No peeling of the coating after water-oxygen corrosion for 300 h, minimum reflectivity of -19.3 dB in the 8-18 GHz band, and infrared emissivity of 0.62 in the 3-5 μm band.
[0254] Comparative Example 4: No peeling of the coating after water-oxygen corrosion for 300 h, minimum reflectivity of -12.3 dB in the 8-18 GHz band, and infrared emissivity of 0.73 in the 3-5 μm band.
[0255] From the test results, it can be seen that the comprehensive performance of the coating of Examples 1-4 is better than that of the coating of Comparative Examples 1-4. The water and oxygen corrosion resistance of Example 1 is better than that of Example 2, which can be due to the higher porosity of the second sub-corrosion-resistant layer in Example 1, which can make the coating have more excellent water and oxygen corrosion resistance. The water and oxygen corrosion resistance of Example 1 is better than that of Comparative Example 1, which can be due to the omission of the dense third sub-corrosion-resistant layer in Comparative Example 1, which will deteriorate the water and oxygen corrosion resistance of the coating. The absolute value of the minimum reflectivity of Example 1 is greater than that of Example 3, which can be due to the lower mass of Ti3SiC2@YSZ in the total mass of Ti3SiC2@YSZ and Al2O3 in Example 1, which can make the coating have more excellent wave absorption performance. The infrared emissivity of Example 1 is lower than that of Example 4, which has more excellent low infrared emissivity characteristics, which can be due to the higher content of noble metal in the infrared stealth layer of Example 1. The absolute value of the minimum reflectivity of Example 1 is greater than that of Comparative Example 2, and the coating of Example 1 has more excellent wave absorption performance, and the wave absorption performance of Comparative Example 2 is extremely poor, which can be due to the use of Ti3SiC2@YSZ material in the second sub-wave absorption layer. The absolute value of the minimum reflectivity of Example 1 is greater than that of Comparative Examples 3 and 4, and the infrared emissivity of Example 1 is lower than that of Comparative Examples 3 and 4. Compared with Comparative Examples 3 and 4, Example 1 has better radar stealth effect and infrared stealth effect. The performance of Comparative Example 3 is poorer, which can be due to the omission of noble metal when preparing the infrared stealth layer of Comparative Example 3. The performance of Comparative Example 4 is poorer, which can be due to the fact that the integrated coating of Comparative Example 4 does not include an infrared stealth layer.
[0256] Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement for part or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.
[0257] Furthermore, to the extent that the terms "comprises", "comprising", "includes", "including" and "has" or any variation thereof are used in the following description and / or claims, such terms are intended to include a non-exclusive inclusion. For example, a process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but can include other elements not expressly listed or inherent to such process, method, article, or apparatus. Also, where appropriate to context, the above description and / or claims can refer to actions to be taken by a person or apparatus. Such actions are sometimes referred to as being taken by an "operator" or "user" where it is contextualually appropriate. However, such actions, or steps, are taken autonomously and automatically by an apparatus, without intervention of a person.
Claims
1. An anticorrosion and radar-infrared compatible stealth function integrated coating, characterized in that, The integrated coating is arranged on a ceramic substrate; The integrated coating comprises a bonding layer, an anti-corrosion layer, a radar wave absorbing layer and an infrared stealth layer arranged in layers, the bonding layer is arranged on the surface of the ceramic substrate; The anti-corrosion layer comprises a first sub-anti-corrosion layer, a second sub-anti-corrosion layer and a third sub-anti-corrosion layer arranged in layers, the first sub-anti-corrosion layer is arranged on the surface of the bonding layer; The material forming the first sub-anti-corrosion layer comprises Yb2Si2O7 and a first pore-forming agent, the mass of the first pore-forming agent accounts for 15-28% of the total mass of Yb2Si2O7 and the first pore-forming agent; The material forming the second sub-anticorrosion layer comprises (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 and a second pore-forming agent, the mass of the second pore-forming agent accounting for 8-18% of the total mass of (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7 and the second pore-forming agent. The material forming the third sub-anticorrosion layer comprises (Yb 0.2 Y 0.2 Er 0.2 Lu 0.2 Sc 0.2 )2Si2O7; The radar wave-absorbing layer comprises a first sub-wave-absorbing layer and a second sub-wave-absorbing layer arranged in layers, the first sub-wave-absorbing layer is arranged on the surface of the corrosion-resistant layer, the material forming the first sub-wave-absorbing layer comprises La 0.7 Sr 0.3 MnO3, Al2O3 and SiO2, and the material forming the second sub-wave-absorbing layer comprises Ti3SiC2@YSZ and Al2O3. The material forming the infrared stealth layer comprises Ti3SiC2 and a noble metal material, the noble metal material comprises at least one of AgPd, Pt and Pd, the mass of the noble metal material accounts for 60-80% of the mass of the material forming the infrared stealth layer.
2. The anti-corrosion and radar-infrared compatible stealth function integrated coating according to claim 1, characterized in that, The anti-corrosion layer satisfies at least one of the following conditions: (1) the thickness of the anti-corrosion layer is 100-250 μm; (2) the thickness of the first sub-anti-corrosion layer is 40-100 μm, the thickness of the second sub-anti-corrosion layer is 40-100 μm, and the thickness of the third sub-anti-corrosion layer is 20-50 μm; (3) the porosity of the first sub-anti-corrosion layer is greater than the porosity of the second sub-anti-corrosion layer, and the porosity of the second sub-anti-corrosion layer is greater than the porosity of the third sub-anti-corrosion layer; (4) the porosity of the first sub-anti-corrosion layer is 20-30%, and the porosity of the second sub-anti-corrosion layer is 15-25%.
3. The corrosion resistant and radar-infrared compatible stealth function integrated coating according to claim 1, characterized in that, The bonding layer satisfies at least one of the following conditions: (1) the material forming the bonding layer comprises Si; (2) the thickness of the bonding layer is 60-110 μm.
4. The corrosion resistant and radar-infrared compatible stealth function integrated coating according to claim 1, characterized in that, The thickness of the radar wave absorbing layer is 700-800 μm.
5. The corrosion resistant and radar-infrared compatible stealth function integrated coating according to claim 4, characterized in that, The radar wave absorbing layer satisfies at least one of the following conditions: (1) the thickness ratio of the first sub-wave absorbing layer to the second sub-wave absorbing layer is 5:4-7:3; (2) in the material forming the first sub-wave-absorbing layer, the La 0.7 Sr 0.3 MnO3 and the mass ratio of the Al2O3, the SiO2 is (1-3):(2-4):5; (3) in the material forming the second sub-wave absorbing layer, the mass of Ti3SiC2@YSZ accounts for (45-65)% of the mass of the material forming the second sub-wave absorbing layer.
6. The corrosion resistant and radar-infrared compatible stealth function integrated coating according to claim 1, characterized in that, The area of the orthographic projection of the infrared stealth layer on the radar wave absorbing layer is less than the area of the radar wave absorbing layer, and the orthographic projection of the infrared stealth layer on the radar wave absorbing layer is a plurality of array-arranged squares; The side length of the square is 0.8-3.5 mm, and the interval distance between adjacent squares is 0.5-1.2 times the side length of the square.
7. The anticorrosion and radar-infrared compatible stealth function integrated coating according to any one of claims 1-6, characterized in that, The thickness of the infrared stealth layer is 20-50 μm.
8. Process for the production of an anti-corrosion and radar-infrared compatible stealth function integrated coating according to any one of claims 1 to 7, characterized in that, It comprises: a bonding layer is formed on the surface of a ceramic substrate by atmospheric plasma spraying; a first sub-anti-corrosion layer and a second sub-anti-corrosion layer are formed on the surface of the bonding layer by atmospheric plasma spraying, and a third sub-anti-corrosion layer is formed on the surface of the second sub-anti-corrosion layer by suspension plasma spraying, the first sub-anti-corrosion layer, the second sub-anti-corrosion layer and the third sub-anti-corrosion layer constitute an anti-corrosion layer; a radar wave absorbing layer is formed on the surface of the anti-corrosion layer; An infrared stealth layer is formed on the surface of the radar wave-absorbing layer by using a suspension supersonic spraying method in combination with a shielding template, and the shielding template is provided with a plurality of square through holes arranged in an array.
9. The method for preparing an anti-corrosion and radar-infrared compatible stealth function integrated coating according to claim 8, characterized in that, Forming a radar wave-absorbing layer on the surface of the anti-corrosion layer comprises: A first sub-wave-absorbing layer is formed on the surface of the anti-corrosion layer by using an atmospheric plasma spraying method. A second sub-wave-absorbing layer is formed on the surface of the first sub-wave-absorbing layer by using a suspension plasma spraying method.
10. The method of claim 9, wherein the method further comprises the step of applying a protective layer on the surface of the radar-infrared compatible stealth coating. The preparation method satisfies at least one of the following conditions: (1) The spraying parameters for forming the bonding layer include: a spraying distance of 130-180 mm, an argon flow rate of 30-40 slpm, a hydrogen flow rate of 6-10 slpm, and a power of 26-35 kW; (2) The spraying parameters for forming the first sub-anti-corrosion layer include: a spraying distance of 100-140 mm, an argon flow rate of 36-47 slpm, a hydrogen flow rate of 8-13 slpm, and a power of 32-42 kW; (3) The spraying parameters for forming the second sub-anti-corrosion layer include: a spraying distance of 100-140 mm, an argon flow rate of 36-47 slpm, a hydrogen flow rate of 8-13 slpm, and a power of 32-42 kW; (4) The spraying parameters for forming the third sub-anti-corrosion layer include: a spraying distance of 50-100 mm, an argon flow rate of 40-50 slpm, a hydrogen flow rate of 6-12 slpm, a liquid feeding flow rate of 40-80 ml / min, and a power of 45-55 kW; (5) The spraying parameters for forming the first sub-wave-absorbing layer include: a spraying distance of 100-140 mm, an argon flow rate of 36-46 slpm, a hydrogen flow rate of 8-12 slpm, and a power of 35-42 kW; (6) The spraying parameters for forming the second sub-wave-absorbing layer include: a spraying distance of 90-130 mm, an argon flow rate of 36-46 slpm, a hydrogen flow rate of 8-12 slpm, a power of 30-40 kW, and a liquid feeding flow rate of 40-60 ml / min; (7) The spraying parameters for forming the infrared stealth layer include: a spraying distance of 150-250 mm, an oxygen pressure of 0.6-1.2 MPa, a hydrogen pressure of 0.4-1.4 MPa, a liquid feeding flow rate of 50-110 ml / min, and a power of 32-40 kW.
Citation Information
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