Ablation-resistant coating as well as preparation and application thereof

Abstract

According to the ablation-resistant coating and the preparation and application thereof, the ablation-resistant temperature and the abrasion-resistant coefficient are increased, and the preparation method comprises the steps that Ti3AlC2 is added into hydrofluoric acid to be fully stirred and washed, then a product is dispersed into distilled water, centrifugal treatment is conducted, and supernatant liquid is obtained; adding micron-sized ZnO into the supernatant liquid, and uniformly stirring to obtain a modified Mexne mixture, wherein the material-liquid ratio is (0.5-0.8) g: 50mL; uniformly mixing the silicon carbide and zirconium carbide mixture with ceramic fibers, and calcining to obtain a modified inorganic filler; chromium sesquioxide is added into the modified Mxene mixture and stirred at a high speed at the temperature of 10-15 DEG C, then the modified inorganic filler continues to be added, the ablation-resistant coating is obtained after uniform stirring, and the material-liquid ratio of the chromium sesquioxide to the modified inorganic filler to the modified Mxene mixture is (0.5-0.8) g: (100-120) g: 100 mL.

Description

Technical Field

[0001] The invention relates to coating technology, and in particular to ablation-resistant coating and preparation and application thereof. Background Art

[0002] The heat flow outlet of the heat flux density meter needs a high temperature resistant coating to protect the thermal sensor. In addition to the traditional ablation resistance function, the coating must also protect the sensitivity of the sensor. Traditional coatings often play a good heat insulation role, resulting in heat loss and reducing the accuracy of the heat flux density meter itself. Summary of the invention

[0003] The present invention is developed in view of the above problems, and its purpose is to provide an ablation-resistant coating with high ablation temperature resistance and wear resistance coefficient and its preparation and application The present invention provides a method for preparing an ablation-resistant coating, comprising: Ti 3 AlC 2 Add to 30%~40% hydrofluoric acid and stir thoroughly for 2h~3h, wherein the solid-liquid ratio is (2~3)g:100mL, and then wash with deionized water-ethanol solution; disperse the treated product in distilled water, wherein the solid-liquid ratio is (3~5)g:100mL, and then place it in a centrifuge for centrifugation at 5000~6000 rpm for 24h~30h to obtain the supernatant; add micron-sized ZnO to the supernatant and stir evenly to obtain a modified Mexne suspension, wherein the solid-liquid ratio is (0.5~0.8)g:50mL; Silicon carbide and zirconium carbide are mixed uniformly in a mass ratio of 1:(1-2), and the silicon carbide-zirconium carbide mixture is further mixed uniformly with ceramic fiber, wherein the mass ratio of the silicon carbide-zirconium carbide mixture to the ceramic fiber is 50:(100-80), and then calcined at a temperature of 800° C. to 1000° C. for 24 h to 30 h to obtain a modified inorganic filler; Chromium trioxide is added to the modified Mxene suspension and stirred at a temperature of 10°C to 15°C and a speed of 5000 to 6000 rpm for 2h to 3h, and then the modified inorganic filler is added and stirred evenly to obtain the ablation-resistant coating, wherein the solid-liquid ratio of the chromium trioxide, the modified inorganic filler and the modified Mxene mixture is (0.5~0.8)g:(100~120)g:100mL.

[0004] The volume ratio of deionized water to ethanol can be 2:(1~1.5).

[0005] Among them, Ti 3 AlC 2 , silicon carbide, zirconium carbide, chromium oxide and ceramic fiber are all powders with a particle size of 10 to 100 microns.

[0006] The present invention also provides an ablation-resistant coating prepared by the above preparation method.

[0007] The present invention further proposes an application of the above-mentioned ablation-resistant coating, comprising applying the coating to a heat measuring part of a heat flux density meter and allowing it to stand and solidify to obtain an ablation-resistant coating.

[0008] Specifically, the heat measuring part is the inner wall through which the heat flow of the heat flux density meter passes. Specifically, it is the inner wall at 0 to 3 cm from the heat flow outlet of the heat flux density meter. Specifically, the coating thickness is 0.8 mm to 1.0 mm.

[0009] According to the present invention, the modified ablation-resistant coating preparation method and its application in a heat flux density meter enhance the adhesion of the inorganic filler through the activation of the silicon polymer by the Mxene-doped silicon carbide and zirconium carbide composite, thereby improving the ablation resistance temperature and the wear resistance coefficient.

[0010] According to the test results, the inventors pointed out that the adhesion of a single-layer MXene and a micron-sized ZnO after mixing is beneficial to thermal stability. The high-melting-point MXene and ZnO are not melted, which can obtain unexpected thermal conductivity and thermal stability. At the same time, the addition of ZnO also plays a role in filling the microscopic holes of the inorganic filler after the coating is cured. At the same time, the doping of chromium trioxide changes the microstructure, which is speculated to be related to the improvement of the efficiency of heat transfer through the coating, thereby enhancing the sensitivity of the sensor and helping to achieve thermal stability. DETAILED DESCRIPTION

[0011] The specific implementation methods of the present invention are used to provide necessary disclosure for those skilled in the art to fully understand the present invention, and are intended to effectively support the claims of the present invention. At the same time, this section will involve the interpretation or definition of the features and terms of the technical solution of the present invention. Those skilled in the art should understand the scope of the claims of the present invention in conjunction with the explanation of the specific features and terms in the specification, and should not arbitrarily distort the true connotations represented by the features and terms of the present invention.

[0012] It must be understood that in any work involving the definition of the scope of the claims of the present invention, the specific embodiments provided by the present invention can be used to fully support the appropriate summaries of equivalent or superior solutions summarized therefrom, and the scope of the claims should never be understood as not exceeding the examples themselves. It must also be understood that with the development of technology and the emergence of new scenarios, the technical solutions provided by the embodiments of the present application will also be applicable to similar technical problems within the scope of those skilled in the art without any creative work, and the scope of protection of the present invention should not be limited to the examples recorded in the specific implementation methods of the present invention.

[0013] The products obtained in the following examples and comparative examples were applied to the following equipment and subjected to temperature stability tests as follows.

[0014] Test method: The coating slurry is applied to 0-3 cm of the heat flow outlet of a heat flux density meter equipped with a GD sensor to obtain an ablation-resistant coating with a coating thickness of 0.8-1.0 mm.

[0015] The following examples and comparative examples are selected from the following materials: Ti 3 AlC 2 , silicon carbide, zirconium carbide, chromium oxide and ceramic fiber are all powders with a particle size of 10 to 100 microns.

[0016] Embodiment 1: 1. Synthesis of micron-sized ZnO-modified Mexne: 2gTi 3 AlC 2 Add 100 mL of 35% hydrofluoric acid by mass, stir thoroughly for 2 hours, wash with a mixed solution of 1000 mL of deionized water and 500 mL of ethanol, then take 3 g of the treated product and add it to 100 mL of distilled water and mix and disperse it evenly, continue to place it in a centrifuge, centrifuge it at 5000 rpm for 24 hours, obtain the supernatant, and then add 0.5 g of micron-grade ZnO to 50 mL of the above-obtained supernatant to obtain a modified Mexne suspension.

[0017] 2. Add 50 g of silicon carbide and zirconium carbide in a mass ratio of 1:1 to 100 g of ceramic fiber and mix evenly. After calcining at 800° C. for 24 hours, return to room temperature to obtain a modified inorganic filler.

[0018] 3. Add 0.5 g of chromium trioxide to 100 mL of modified Mxene suspension, stir at high speed (5000 rpm) at 10 °C for 2 h, then return to room temperature. Continue to add 100 g of modified inorganic filler, stir evenly, and return to room temperature to obtain a coating slurry.

[0019] Performance Testing: 1. Ablation resistance temperature 1590℃ 2. Wear resistance after high temperature: Wear value: 3g / 100r 3. The difference between the temperature measured by the sensor and the actual temperature is less than 15°C.

[0020] 4. Thermal stability of the coating: Weight loss rate after calcination at 800°C for 10 minutes: 0.75%.

[0021] Embodiment 2: 1. Synthesis of micron-sized ZnO-modified Mexne: 3gTi 3 AlC 2 Add 100 mL of 35% hydrofluoric acid by mass, stir thoroughly for 3 h, wash with a mixed solution of 1000 mL of deionized water and 750 mL of ethanol, then take 4 g of the treated product and add it to 100 mL of distilled water and mix and disperse it evenly, continue to place it in a centrifuge, centrifuge it at 6000 rpm for 30 h, obtain the supernatant, and then add 0.8 g of micron-grade ZnO to 50 mL of the above-obtained supernatant to obtain a modified Mexne suspension.

[0022] 2. Add 50 g of silicon carbide and zirconium carbide in a mass ratio of 1:2 to 80 g of ceramic fiber and mix evenly. After calcining at 1000° C. for 30 hours, return to room temperature to obtain a modified inorganic filler.

[0023] 3. Add 0.8 g of chromium trioxide to 100 mL of modified Mxene suspension, stir at high speed (5000 rpm) at 15 °C for 3 h, then return to room temperature, add 120 g of modified inorganic filler, stir evenly to obtain coating slurry.

[0024] Performance Testing: 1. Ablation resistance temperature 1510℃ 2. Wear resistance after high temperature: Wear value: 3.1g / 100r 3. The difference between the temperature measured by the sensor and the actual temperature is less than 17°C.

[0025] 4. Thermal stability of the coating: Weight loss rate after calcination at 800°C for 10 minutes: 0.98%.

[0026] Comparative Example 1: 1. Synthesis of Mexne: 2gTi 3 AlC 2 Add 100 mL of 35% hydrofluoric acid, stir thoroughly for 2 h, wash with a mixed solution of 1000 mL of deionized water and 500 mL of ethanol, then take 3 g of the treated product and add it to 100 mL of distilled water and mix and disperse evenly, continue to place it in a centrifuge, centrifuge it at 5000 rpm for 24 h, and take the supernatant to obtain the Mxene suspension.

[0027] 2. Add 50 g of silicon carbide and zirconium carbide in a mass ratio of 1:1 to 100 g of ceramic fiber and mix evenly. After calcining at 800° C. for 24 hours, return to room temperature to obtain a modified inorganic filler.

[0028] 3. Add 0.5 g of chromium trioxide to 100 mL of Mxene aqueous solution, stir at high speed (5000 rpm) at 10 ° C for 2 hours, then return to room temperature, continue to add 100 g of modified inorganic filler, stir evenly to obtain a coating slurry.

[0029] test: 1. Ablation resistance temperature 1010℃ 2. Wear resistance after high temperature: Wear value: 6.2g / 100r 3. The difference between the temperature measured by the sensor and the actual temperature is less than 48°C.

[0030] 4. Thermal stability of the coating: Weight loss rate after calcination at 800°C for 10 minutes: 1.25%.

[0031] Comparative Example 2: 1. Synthesis of micron-sized ZnO-modified Mexne: 2gTi 3 AlC 2 Add 100 mL of 35% hydrofluoric acid by mass, stir thoroughly for 2 hours, wash with a mixed solution of 1000 mL of deionized water and 500 mL of ethanol, then take 3 g of the treated product and add it to 100 mL of distilled water and mix and disperse it evenly, continue to place it in a centrifuge, centrifuge it at 5000 rpm for 24 hours, obtain the supernatant, and then add 0.5 g of micron-grade ZnO to 50 mL of the above-obtained supernatant to obtain a modified Mexne suspension.

[0032] 2. Add 50 g of silicon carbide and zirconium carbide in a mass ratio of 1:1 to 100 g of ceramic fiber and mix evenly. After calcining at 800° C. for 24 hours, return to room temperature to obtain a modified inorganic filler.

[0033] 3. Add 100 g of modified inorganic filler to 100 mL of modified MXene suspension, stir evenly at room temperature to obtain coating slurry.

[0034] Performance Testing: 1. Ablation resistance temperature 1410℃ 2. Wear resistance after high temperature: Wear value: 4.4g / 100r 3. The difference between the temperature measured by the sensor and the actual temperature is less than 45°C.

[0035] 4. Thermal stability of the coating: Weight loss rate after calcination at 800°C for 10 minutes: 2.23%.

[0036] Application examples: The coating obtained in Example 1-2 was applied to the inner wall of the heat flow outlet of the heat flux density meter at 0-3 cm, and after standing and curing, an ablation-resistant coating was obtained, and the coating thickness was 0.8 mm-1.0 mm.

Claims

1. A method for preparing an ablation-resistant coating, characterized in that: The preparation method comprises: Ti3AlC2 was added to hydrofluoric acid with a mass fraction of 30% to 40% and stirred for 2h to 3h, wherein the solid-liquid ratio was (2~3) g:100mL, and then washed with a deionized water-ethanol solution; the treated product was dispersed in distilled water, wherein the solid-liquid ratio was (3~5) g:100mL, and then placed in a centrifuge for centrifugation at a speed of 5000~6000 rpm for 24h to 30h to obtain a supernatant; micron-sized ZnO was added to the supernatant and stirred evenly to obtain a modified Mexne suspension, wherein the solid-liquid ratio was (0.5~0.8) g:50mL; Silicon carbide and zirconium carbide are mixed uniformly in a mass ratio of 1:(1-2), and the silicon carbide-zirconium carbide mixture is further mixed uniformly with ceramic fiber, wherein the mass ratio of the silicon carbide-zirconium carbide mixture to the ceramic fiber is 50:(100-80), and then calcined at a temperature of 800° C. to 1000° C. for 24 h to 30 h to obtain a modified inorganic filler; Chromium trioxide is added to the modified Mxene mixture and stirred at a temperature of 10°C to 15°C and a speed of 5000 to 6000 rpm for 2h to 3h, and then the modified inorganic filler is added and stirred evenly to obtain the ablation-resistant coating, wherein the solid-liquid ratio of chromium trioxide, modified inorganic filler and modified Mxene suspension is (0.5~0.8) g: (100~120) g: 100 mL.

2. The preparation method according to claim 1, wherein The volume ratio of deionized water and ethanol is 2:(1~1.5).

3. The preparation method according to claim 1, wherein Ti3AlC2, silicon carbide, zirconium carbide, chromium oxide and ceramic fiber are all powders with a particle size of 10 to 100 microns.

4. An ablation-resistant coating prepared by the preparation method according to any one of claims 1 to 3.

5. An application of the ablation-resistant coating according to claim 4, characterized in that: The coating is applied to the heat measuring part of the heat flux density meter and left to stand and solidify to obtain the ablation-resistant coating.

6. The use according to claim 5, wherein: The heat measuring part is the heat flux of the heat flux density meter passing through the inner wall.

7. The use according to claim 5, wherein: The heat measuring part is the inner wall at 0-3 cm from the heat flow outlet of the heat flux density meter.

8. The use according to claim 5, wherein: The coating thickness is 0.8mm~1.0mm.