High-temperature-resistant multi-spectrum compatible stealth material and preparation method thereof

Abstract

The application provides a high-temperature-resistant multi-frequency spectrum compatible stealth material and a preparation method thereof. The stealth material comprises a substrate layer, a first functional layer and a second functional layer. The first functional layer is located on the upper surface of the substrate layer, and the second functional layer is located on the upper surface of the first functional layer. The second functional layer is a titanium dioxide layer with uneven thickness, and the second functional layer comprises at least two thickness modules with different thicknesses. The first functional layer plays a main infrared wave band stealth function, the second functional layer is designed as an uneven thickness structure, and through the thickness design, different structural colors are exhibited in the visible light wave band, the visible light wave band stealth function is realized, the infrared wave band stealth is considered at the same time, and the stable work under high temperature can be realized.

Description

Technical Field

[0001] This invention relates to the field of stealth materials technology, and more specifically, to a high-temperature resistant, multi-spectral compatible stealth material and its preparation method. Background Technology

[0002] With the rapid development of infrared detection and guidance technologies and the continuous improvement of detection accuracy, stealth technology has attracted great attention from countries around the world in areas such as aircraft, ground weapons and equipment, and strategic and tactical missiles. Currently, reducing the surface temperature and emissivity of targets are the main means of achieving infrared stealth. However, for high-temperature components such as engines or aircraft, reducing the surface temperature of targets is very difficult, making low emissivity an important direction for the development of infrared stealth.

[0003] Current infrared stealth materials typically use metal powder as filler to prepare coatings or thin films on a substrate. The primary metal powder used is aluminum powder, which possesses excellent electrical conductivity and low emissivity. However, during high-speed flight, the surface temperature of an aircraft rises dramatically (>800℃), and its infrared radiation intensity increases by orders of magnitude. This poses a significant challenge to stealth in the infrared band. Furthermore, aluminum has a melting point of around 600℃, and organic binders have even worse temperature resistance, easily oxidizing and decomposing at high temperatures. Therefore, low-emissivity coatings cannot meet the stringent temperature requirements. In addition to infrared stealth, stealth in the visible light range is also crucial; however, the luster of metals results in poor stealth performance in the visible light range. Moreover, the fabrication process of metal thin-film stealth materials is relatively complex, and film agglomeration occurs at high temperatures, making it difficult to reconcile infrared and visible light stealth performance, thus failing to meet the needs of practical applications.

[0004] Therefore, there is an urgent need in this field for a stealth material that can operate stably at high temperatures and simultaneously achieve stealth in both the infrared and visible light bands, in order to meet the performance requirements of increasingly sophisticated weapons and aerospace vehicles. Summary of the Invention

[0005] This invention provides a high-temperature resistant, multi-spectral compatible stealth material and its preparation method to solve the problems of poor stealth performance in high-temperature environments, inability to meet high-temperature requirements, inability to work stably in high-temperature environments, and inability to simultaneously achieve stealth in both infrared and visible light bands.

[0006] On one hand, the present invention provides a high-temperature resistant, multi-spectral compatible stealth material, comprising a substrate layer, a first functional layer, and a second functional layer, wherein the first functional layer is located on the upper surface of the substrate layer, and the second functional layer is located on the upper surface of the first functional layer; the second functional layer is a titanium dioxide layer with uneven thickness, and the second functional layer comprises at least two thickness modules with different thicknesses.

[0007] Compared with the prior art, the present invention has the following beneficial effects: the first functional layer of the present invention plays the main infrared band stealth function, and the second functional layer is designed with a non-uniform thickness structure. Through the thickness design, different structural colors are displayed in the visible light band, realizing the visible light band stealth function, while also taking into account the infrared band stealth, and can work stably at high temperatures.

[0008] In some embodiments of the present invention, the substrate layer is a silicon wafer substrate or a nickel-based alloy substrate; the first functional layer is a zirconium boride layer with uniform thickness, and the thickness of the first functional layer is 300-500 nm.

[0009] The beneficial effects of adopting the above-mentioned further technical solution are that the first functional layer of the present invention is a zirconium boride layer with uniform thickness of 300-500nm, and the second functional layer is a titanium dioxide layer with uneven thickness. Compared with traditional metal films and semiconductor coatings, the stealth material of the present invention, through the dual-functional layer design, has a temperature resistance of over 1000℃. Compared with the temperature resistance of traditional coatings and films of <600℃, it has excellent high temperature resistance and stability, can be used at high temperatures above 1000℃, and has low infrared emissivity (≤0.2), good stealth effect, avoids the problems of poor temperature resistance and easy oxidation and decomposition of organic adhesives at high temperatures, and does not exhibit agglomeration at high temperatures, thus taking into account both infrared stealth performance and visible light stealth performance.

[0010] In some embodiments of the present invention, the thickness of the thickness modules of the second functional layer of different thicknesses is selected from 10-1000 nm.

[0011] The beneficial effect of adopting the above-mentioned further technical solution is that the second functional layer of the present invention includes thickness modules of different thicknesses, and the thickness of the thickness modules of different thicknesses is selected from 10-1000nm. In the visible light band, the thickness of the thickness modules of different thicknesses can be designed in the range of 10-1000nm according to the application environment, so that the second functional layer displays a structural color similar to or consistent with the application environment (for example, a thickness module of 50nm displays blue, a thickness module of 170nm displays green, and a thickness module of 200nm displays yellow), blending into the environment and achieving stealth in the visible light band, thereby achieving multi-spectral stealth in visible light-near infrared-mid and far infrared.

[0012] In some embodiments of the present invention, the number of thickness modules of any thickness of the second functional layer is at least one. When the number of thickness modules of any thickness of the second functional layer is not less than two, the thickness modules are randomly distributed or interleaved.

[0013] The beneficial effect of adopting the above-mentioned further technical solution is that the present invention adapts to different environments by distributing thickness modules of different thicknesses, and can reasonably adjust the color rendering according to the application environment to blend into the environment, thereby achieving stealth in the visible light band, and further achieving multi-spectral stealth in visible light-near infrared-mid and far infrared.

[0014] On the other hand, the present invention also provides a method for preparing the high-temperature resistant multi-spectral compatible stealth material according to any one of the above claims, comprising the following steps: S1, pretreating the substrate; S2, sputtering a first functional layer on the upper surface of the pretreated substrate; S3, sputtering a second functional layer on the upper surface of the first functional layer to obtain a high-temperature resistant multi-spectral compatible stealth material blank; S4, heat-treating the high-temperature resistant multi-spectral compatible stealth material blank to obtain the high-temperature resistant multi-spectral compatible stealth material.

[0015] Compared with the prior art, the present invention has the following beneficial effects: The present invention obtains a stealth material blank by sequentially preparing a first functional layer and a second functional layer on the upper surface of the substrate. After heat treatment, the adhesion between the substrate layer, the first functional layer and the second functional layer can be improved, delamination can be prevented, and a stealth material with strong interlayer bonding force, which can achieve stealth in both infrared and visible light bands and can work stably at high temperatures can be obtained.

[0016] In some embodiments of the present invention, the pretreatment includes: cleaning the substrate with deionized water, ultrasonically cleaning the substrate with anhydrous ethanol, and drying the substrate to obtain the pretreated substrate.

[0017] The beneficial effect of adopting the above-mentioned further technical solution is that by pretreating the substrate to maintain the surface state of the substrate, it is beneficial to improve the adhesion of the first functional layer to the substrate layer.

[0018] In some embodiments of the present invention, the specific process of step S2 is as follows: the pretreated substrate is placed on a magnetron sputtering deposition stage; a ZrB2 target is used as the magnetron sputtering target, and the target-substrate distance is set to 100-500 nm, at a value below 5 × 10⁻⁶ nm. -4 Under a vacuum background of Pa, argon gas is introduced into the sputtering chamber at a gas flow rate of 25-35 L / min until the sputtering pressure is 0.8-2 Pa. Pre-sputtering is performed for 2-20 min at a sputtering power of 100-400 W and a sputtering rate of 10-50 nm / min. After pre-sputtering, sputtering is performed for 5-10 min at a sputtering rate of 10-50 nm / min under the conditions of sputtering power of 100-400 W, sputtering pressure of 0.2-0.9 Pa, and deposition temperature of room temperature to obtain a first functional layer with uniform thickness.

[0019] The beneficial effect of adopting the above-mentioned further technical solution is that, through the design of magnetron sputtering parameters, the present invention first performs pre-sputtering on the substrate to improve the adhesion of the first functional layer on the substrate layer. Then, with the further design of magnetron sputtering parameters, a first functional layer with uniform thickness can be obtained, which has excellent properties such as low infrared emissivity, impact resistance, high adhesion, and high temperature resistance.

[0020] In some embodiments of the present invention, the specific process of step S3 is as follows: S31, the substrate sputtered with the first functional layer is taken out from the sputtering cavity, and according to the preset thickness module distribution state of the second functional layer, the thick module distribution area is shielded by a shielding mold, and then placed on the magnetron sputtering deposition stage; S32, using Ti target as the magnetron sputtering target, the target-substrate distance is set to 100-500nm, and the distance is below 5×10 -4 Under a vacuum of 0.8 Pa, argon and reactive gas O2 are introduced into the sputtering chamber at a gas flow rate of 20-50 L / min until the sputtering pressure is 0.8-2 Pa. Sputtering is performed at a sputtering rate of 10-50 nm / min under conditions of sputtering power of 80-150 W and deposition temperature of 280-400 °C until the sputtered thickness is the preset thickness of the unshielded thickness module minus the preset compensation thickness. S33: Remove the sputtered product from the sputtering chamber after S32 and remove the shielding mold from the lower thickness distribution area of ​​the unsputtered thickness module distribution area. According to the preset thickness module distribution state of the second functional layer, the thick modules that have been sputtered and the high-thickness distribution areas of different thickness module distribution areas that have not been sputtered are shielded by shielding molds. After shielding, the substrate is placed on a magnetron sputtering deposition stage. S34. Repeat steps S32 and S33 until all the preset thickness modules of the second functional layer have been sputtered. S35. Remove all shielding molds, place the substrate on a magnetron sputtering deposition stage, and perform sputtering with preset compensation thickness according to the sputtering parameters in step S32. After sputtering, a high-temperature resistant multi-spectral compatible stealth material preform is obtained.

[0021] The beneficial effects of adopting the above-mentioned further technical solution are as follows: This invention involves stepwise fabrication of thickness modules of different thicknesses of the second functional layer on the first functional layer. The process is simple, and with the design of magnetron sputtering parameters, coupled with the relatively small thickness of the second functional layer itself, the junctions of the thickness modules of different thicknesses are smoothly transitioned, avoiding large abrupt changes in thickness angle. Furthermore, when fabricating thickness modules of different thicknesses stepwise, a preset compensation thickness is reserved during sputtering. By uniformly sputtering with the preset compensation thickness, any abrupt thickness changes that may exist at the junctions of the thickness modules of different thicknesses are eliminated, resulting in a smooth outer surface of the entire second functional layer, which is beneficial for color development in the visible light band.

[0022] In some embodiments of the present invention, the shielding mold is a metal mold or an organic film mold; in step S32, the volume ratio of argon to O2 is (5:1)-(12:1); the preset compensation thickness is 5-10 nm.

[0023] The beneficial effects of adopting the above-mentioned further technical solutions are that the metal mold or organic film mold, especially the organic film mold, has a better shielding effect and is less likely to cause thickness abrupt changes or film layer expansion at the junction of different thickness modules; the volume ratio of argon to O2 is (5:1)-(12:1), which is conducive to the sputtering of the second functional layer; and the preset compensation thickness of 5-10nm is sufficient to eliminate the possible thickness abrupt changes at the junction of different thickness modules.

[0024] In some embodiments of the present invention, the heat treatment includes: heating from room temperature to 760-820°C at a heating rate of 2-6°C / min under vacuum, holding at that temperature for 1-3 hours, and then cooling to room temperature at a cooling rate of 3-5°C / min.

[0025] The beneficial effect of adopting the above-mentioned further technical solution is that, based on the sputtering of TiO2 / ZrB2 dual-layer functional layers, the present invention designs the heat treatment parameters, which is conducive to improving the adhesion between layers. Detailed Implementation

[0026] To make the objectives, technical solutions and advantages of the present invention clearer, the various aspects of the present invention will be described in detail below with reference to specific embodiments. However, these specific embodiments are only used to illustrate the present invention and do not constitute any limitation on the scope of protection and the substantive content of the present invention.

[0027] Example 1:

[0028] This embodiment provides a high-temperature resistant, multi-spectral compatible stealth material, including a substrate layer, a first functional layer, and a second functional layer. The first functional layer is located on the upper surface of the substrate layer, and the second functional layer is located on the upper surface of the first functional layer. The second functional layer is a titanium dioxide layer with uneven thickness, and the second functional layer includes at least two thickness modules with different thicknesses.

[0029] In this embodiment, the substrate is a silicon wafer substrate or a nickel-based alloy substrate. Specifically, the nickel-based alloy substrate is a K424 nickel-based high-temperature alloy substrate. This embodiment does not have a specific limitation on the source of the K424 nickel-based high-temperature alloy substrate; any commercially available alloy of the corresponding grade can be used. The first functional layer is a zirconium boride layer with uniform thickness, ranging from 300 to 500 nm. In this embodiment, uniform thickness means that the thickness of the first functional layer is consistent or slightly different across different parts, with the difference being within 5 nm (for example, if the thickness of the first functional layer falls within the range of 300 ± 5 nm, it is considered that the thickness of the first functional layer is 300 nm).

[0030] In this embodiment, preferably, the thickness of the thickness modules of different thicknesses in the second functional layer is selected from 10-1000nm. That is, although the thickness of each thickness module is different, the thickness is selected from 10-1000nm (for example, when the second functional layer includes three thickness modules of different thicknesses, the thickness of the first thickness module is 10nm, the thickness of the second thickness module is 50nm, and the thickness of the third thickness module is 100nm. The thicknesses are different but all are selected from 10-1000nm. In addition, the specific thickness includes the thickness within a certain difference, which can be 2nm. For example, the thickness range is considered to be the first thickness module if it is within 10±2nm).

[0031] In this embodiment, the number of thickness modules of any thickness in the second functional layer is at least one. When the number of thickness modules of any thickness in the second functional layer is not less than two, the thickness modules are randomly distributed or interleaved (for example, if the second functional layer includes three different thickness modules and the number of each thickness module is two, there are a total of six thickness modules, which are randomly distributed or interleaved). In this embodiment, the distribution of thickness modules of different thicknesses can be adjusted according to the actual application environment to ensure that the color rendering is similar to or consistent with the environment, thereby achieving the effect of blending into the environment and becoming invisible.

[0032] This embodiment also provides a method for preparing the high-temperature resistant, multi-spectral compatible stealth material of this embodiment, including the following steps:

[0033] S1. Pre-treat the substrate; specifically, the pre-treatment includes: cleaning the substrate with deionized water, then ultrasonically cleaning the substrate with anhydrous ethanol, and drying the substrate to obtain the pre-treated substrate.

[0034] S2. Sputter the first functional layer onto the pretreated substrate surface; the specific process is as follows: Place the pretreated substrate on a magnetron sputtering deposition stage; use a ZrB2 target with a diameter of 100 mm and a purity of 99.99% as the magnetron sputtering target, set the target-substrate distance to 100-500 nm, and maintain a distance below 5 × 10⁻⁶ nm. -4 Under a vacuum background of Pa, 99.99% pure argon gas is introduced into the sputtering chamber at a gas flow rate of 25-35 L / min until the sputtering pressure is 0.8-2 Pa. Pre-sputtering is performed for 2-20 min at a sputtering power of 100-400 W and a sputtering rate of 10-50 nm / min. After pre-sputtering, sputtering is performed for 5-10 min at a sputtering rate of 10-50 nm / min under the conditions of sputtering power of 100-400 W, sputtering pressure of 0.2-0.9 Pa, and deposition temperature of room temperature to obtain a first functional layer with uniform thickness of 300-500 nm.

[0035] S3. Sputter a second functional layer onto the surface of the first functional layer to obtain a high-temperature resistant, multi-spectral compatible stealth material preform. The specific process is as follows: S31. Remove the substrate with the first functional layer sputtered from the sputtering chamber. According to the preset thickness module distribution of the second functional layer, use a metal mold or organic film mold as a shielding mold to shield the high-thickness module distribution area. After shielding, place it on a magnetron sputtering deposition stage. S32. Use a Ti target with a diameter of 100 mm and a purity of 99.99% as the magnetron sputtering target. Set the target-substrate distance to 100-500 nm. -4 Under a vacuum background of Pa, argon gas with a purity of 99.99% and reactive gas O2 with a purity of 99.997% (volume ratio of 5:1)-(12:1) are introduced into the sputtering chamber at a gas flow rate of 20-50 L / min until the sputtering pressure is 0.8-2 Pa. Sputtering is performed at a sputtering rate of 10-50 nm / min under conditions of sputtering power of 80-150 W, deposition temperature (substrate temperature) of 280-400 °C, and by controlling the deposition time until the sputtered thickness is the preset thickness of the unshielded thickness module minus the preset compensation thickness (e.g., the preset compensation thickness is 5-10 nm). S33: Remove the sputtered product from the sputtering chamber after S32, and remove the low-thickness parts from the different thickness module distribution areas that were not sputtered. The shielding mold on the thickness module distribution area is used to shield the high-thickness thickness module distribution area in the already sputtered thickness module and the unsputtered thickness module distribution area in the different thickness module distribution areas according to the preset thickness module distribution state of the second functional layer. After shielding, it is placed on the magnetron sputtering deposition stage; S34, repeat steps S32 and S33 until all the preset thickness modules of the second functional layer are sputtered; S35, remove all shielding molds, place on the magnetron sputtering deposition stage, and perform sputtering with preset compensation thickness according to the sputtering parameters in step S32. After sputtering, a high-temperature multi-spectral compatible stealth material preform with non-mirror reflection low infrared emissivity TiO2 / ZrB2 double layer film with multiple colors and infrared stealth characteristics is obtained.

[0036] S4. Heat treatment is performed on the high-temperature resistant multi-spectral compatible stealth material billet. The heat treatment includes: placing the high-temperature resistant multi-spectral compatible stealth material billet in a tube furnace and evacuating the furnace until the gas pressure inside the tube reaches 5×10⁻⁶. -4 Pa, under vacuum, is heated from room temperature to 760-820℃ at a heating rate of 2-6℃ / min and held at that temperature for 1-3 hours, and then cooled to room temperature at a cooling rate of 3-5℃ / min to obtain a high-temperature resistant multi-spectral compatible stealth material.

[0037] Example 2:

[0038] This embodiment provides a high-temperature resistant, multi-spectral compatible stealth material, including a substrate layer, a first functional layer, and a second functional layer. The first functional layer is located on the upper surface of the substrate layer, and the second functional layer is located on the upper surface of the first functional layer. The second functional layer is a titanium dioxide layer with uneven thickness, and the second functional layer includes two thickness modules with different thicknesses.

[0039] In this embodiment, the substrate is a silicon wafer. The first functional layer is a zirconium boride layer with uniform thickness, and the thickness of the first functional layer is 300 nm. In this embodiment, uniform thickness means that the thickness of each part of the first functional layer is the same or slightly different, and the difference can be within 5 nm (that is, the thickness of the first functional layer is considered to be 300 nm if it falls within 300 ± 5 nm).

[0040] In this embodiment, preferably, the two thickness modules of the second functional layer with different thicknesses are a first thickness module with a thickness of 10nm and a second thickness module with a thickness of 50nm. In addition, the thickness range of 10±2nm is also classified as the first thickness module of 10nm, and the thickness range of 50±2nm is also classified as the second thickness module of 50nm.

[0041] In this embodiment, the number of thickness modules of any thickness in the second functional layer is at least one. When the number of thickness modules of any thickness in the second functional layer is not less than two, the thickness modules are randomly distributed or interleaved (for example, if the second functional layer includes two thickness modules of different thicknesses and the number of each thickness module is two, there are a total of four thickness modules, which are randomly distributed or interleaved). In this embodiment, the distribution of thickness modules of different thicknesses can be adjusted according to the actual application environment to ensure that the color rendering is similar to the environment, thereby achieving the effect of blending into the environment and becoming invisible.

[0042] This embodiment also provides a method for preparing the high-temperature resistant, multi-spectral compatible stealth material of this embodiment, including the following steps:

[0043] S1. Pre-treat the substrate; specifically, the pre-treatment includes: cleaning the substrate with deionized water, then ultrasonically cleaning the substrate with anhydrous ethanol, and drying the substrate to obtain the pre-treated substrate.

[0044] S2. Sputter the first functional layer onto the pretreated substrate surface; the specific process is as follows: Place the pretreated substrate on a magnetron sputtering deposition stage; use a ZrB2 target with a diameter of 100 mm and a purity of 99.99% as the magnetron sputtering target, set the target-substrate distance to 100 nm, and set the sputtering distance to below 5 × 10⁻⁶ nm. -4Under a vacuum background of Pa, 99.99% pure argon gas was introduced into the sputtering chamber at a gas flow rate of 25 L / min until the sputtering pressure was 0.8 Pa. Pre-sputtering was performed for 2 min at a sputtering power of 400 W and a sputtering rate of 10 nm / min. After pre-sputtering, sputtering was performed for 5 min at a sputtering rate of 10 nm / min under the conditions of sputtering power of 400 W, sputtering pressure of 0.2 Pa, and deposition temperature of room temperature to obtain a first functional layer with uniform thickness of 300 nm.

[0045] S3. Sputter a second functional layer onto the surface of the first functional layer to obtain a high-temperature resistant, multi-spectral compatible stealth material preform. The specific process is as follows: S31. Remove the substrate with the first functional layer sputtered from the sputtering cavity. According to the preset thickness module distribution of the second functional layer, use a metal mold as a shielding mold to shield the high-thickness thickness module distribution area (the second thickness module distribution area). After shielding, place it on a magnetron sputtering deposition stage. S32. Use a Ti target with a diameter of 100 mm and a purity of 99.99% as the magnetron sputtering target. Set the target-substrate distance to 100 nm. [The remaining text appears to be incomplete and requires further context.] -4 Under a vacuum of 0.8 Pa, argon gas with a purity of 99.99% and reactive gas O2 with a purity of 99.997% (volume ratio 5:1) are introduced into the sputtering chamber at a gas flow rate of 20 L / min until the sputtering pressure reaches 0.8 Pa. Sputtering is performed at a sputtering power of 150 W, a deposition temperature (substrate temperature) of 280 °C, and a sputtering rate of 10 nm / min. The deposition time is controlled until the sputtered thickness reaches the preset thickness of the unshielded thickness module minus the preset compensation thickness (e.g., the preset compensation thickness is 5 nm). S33: The sputtered product after S32 is removed from the sputtering chamber, and the unsputtered thickness is removed. The shielding mold on the module distribution area (second thickness module distribution area) shields the sputtered thickness module (first thickness module) according to the preset thickness module distribution state of the second functional layer. After shielding, it is placed on the magnetron sputtering deposition stage; S34, repeat step S32; S35, remove all shielding molds, place on the magnetron sputtering deposition stage, and perform sputtering with preset compensation thickness according to the sputtering parameters of step S32. After sputtering, a high-temperature multi-spectral compatible stealth material preform with non-mirror reflection low infrared emissivity TiO2 / ZrB2 double layer film with two colors and infrared stealth characteristics is obtained.

[0046] S4. Heat treatment is performed on the high-temperature resistant multi-spectral compatible stealth material billet. The heat treatment includes: placing the high-temperature resistant multi-spectral compatible stealth material billet in a tube furnace and evacuating the furnace until the gas pressure inside the tube reaches 5×10⁻⁶. -4Pa, under vacuum, was heated from room temperature to 760°C at a heating rate of 2°C / min and held at that temperature for 3 hours. Then, it was cooled back to room temperature at a cooling rate of 3°C / min to obtain a high-temperature resistant multi-spectral compatible stealth material.

[0047] Example 3:

[0048] This embodiment provides a high-temperature resistant, multi-spectral compatible stealth material, including a substrate layer, a first functional layer, and a second functional layer. The first functional layer is located on the upper surface of the substrate layer, and the second functional layer is located on the upper surface of the first functional layer. The second functional layer is a titanium dioxide layer with uneven thickness, and the second functional layer includes three thickness modules with different thicknesses.

[0049] In this embodiment, the substrate is a nickel-based alloy substrate, specifically a K424 nickel-based high-temperature alloy substrate. This embodiment does not have a specific limitation on the source of the K424 nickel-based high-temperature alloy substrate; any commercially available alloy of the corresponding grade can be used. The first functional layer is a uniformly thick zirconium boride layer with a thickness of 400 nm. In this embodiment, uniform thickness means that the thickness of the first functional layer is consistent or slightly different across different parts, with the difference being within 5 nm (for example, the thickness of the first functional layer falling within the range of 400 ± 5 nm is considered to be 400 nm).

[0050] In this embodiment, the three thickness modules of the second functional layer with different thicknesses are thickness module a with a thickness of 900nm, thickness module b with a thickness of 950nm, and thickness module c with a thickness of 1000nm. In addition, thickness modules with a thickness range of 900±2nm are also classified as thickness module a, thickness modules with a thickness range of 950±2nm are also classified as thickness module b, and thickness modules with a thickness range of 1000±2nm are also classified as thickness module c.

[0051] In this embodiment, the number of thickness modules of any thickness in the second functional layer is at least one. When the number of thickness modules of any thickness in the second functional layer is not less than two, the thickness modules are randomly distributed or interleaved (for example, if the second functional layer includes three different thickness modules and the number of each thickness module is two, there are a total of six thickness modules, which are randomly distributed or interleaved). In this embodiment, the distribution of thickness modules of different thicknesses can be adjusted according to the actual application environment to ensure that the color rendering is similar to the environment, achieving the effect of blending into the environment and becoming invisible.

[0052] This embodiment also provides a method for preparing the high-temperature resistant, multi-spectral compatible stealth material of this embodiment, including the following steps:

[0053] S1. Pre-treat the substrate; specifically, the pre-treatment includes: cleaning the substrate with deionized water, then ultrasonically cleaning the substrate with anhydrous ethanol, and drying the substrate to obtain the pre-treated substrate.

[0054] S2. Sputter the first functional layer onto the pretreated substrate surface; the specific process is as follows: Place the pretreated substrate on a magnetron sputtering deposition stage; use a ZrB2 target with a diameter of 100 mm and a purity of 99.99% as the magnetron sputtering target, set the target-substrate distance to 350 nm, and maintain a speed below 5 × 10⁻⁶ nm. -4 Under a vacuum background of Pa, 99.99% pure argon gas was introduced into the sputtering chamber at a gas flow rate of 30 L / min until the sputtering pressure reached 1.0 Pa. Pre-sputtering was performed for 5 min at a sputtering power of 300 W and a sputtering rate of 30 nm / min. After pre-sputtering, sputtering was performed at a sputtering power of 300 W, a sputtering pressure of 0.5 Pa, and a deposition temperature of room temperature at a sputtering rate of 25 nm / min for 7 min to obtain a first functional layer with uniform thickness and a thickness of 400 nm.

[0055] S3. Sputter a second functional layer onto the surface of the first functional layer to obtain a high-temperature resistant, multi-spectral compatible stealth material preform. The specific process is as follows: S31. Remove the substrate with the first functional layer sputtered from the sputtering cavity. According to the preset thickness module distribution of the second functional layer, use an organic film mold as a shielding mold to shield the thickness module b and thickness module c distribution areas. After shielding, place it on a magnetron sputtering deposition stage. S32. Use a Ti target with a diameter of 100 mm and a purity of 99.99% as the magnetron sputtering target, set the target-substrate distance to 350 nm, and set the target distance to less than 5 × 10⁻⁶ nm. -4Under a vacuum background of Pa, argon gas with a purity of 99.99% and reactive gas O2 with a purity of 99.997% (volume ratio 9:1) are introduced into the sputtering chamber at a gas flow rate of 25 L / min until the sputtering pressure reaches 1.2 Pa. Sputtering is performed at a sputtering rate of 25 nm / min under conditions of sputtering power of 100 W, deposition temperature (substrate temperature) of 350 °C, and the deposition time is controlled until the sputtered thickness is the preset thickness of the unshielded thickness module minus the preset compensation thickness (e.g., the preset compensation thickness is 8 nm). S33: The sputtered product after S32 is removed from the sputtering chamber, and the shielding mold on the low-thickness thickness module b distribution area in the unsputtered thickness module b distribution area and the thickness module c distribution area is removed. According to the preset thickness module distribution state of the second functional layer, The sputtered thickness module a and the unsputtered thickness module c are shielded using a shielding mold. After shielding, the module is placed on a magnetron sputtering deposition stage. S34. Repeat S32. After sputtering, the module is removed and the shielding mold on the unsputtered thickness module c is removed. According to the preset thickness module distribution state of the second functional layer, the sputtered thickness modules a and b are shielded using a shielding mold. After shielding, the module is placed on a magnetron sputtering deposition stage and S32 is repeated. S35. Remove all shielding molds and place the module on a magnetron sputtering deposition stage. Sputtering with preset compensation thickness is performed according to the sputtering parameters in step S32. After sputtering, a high-temperature multi-spectral compatible stealth material preform with non-mirror reflection and low infrared emissivity TiO2 / ZrB2 double-layer film with three colors and infrared stealth characteristics is obtained.

[0056] S4. Heat treatment is performed on the high-temperature resistant multi-spectral compatible stealth material billet. The heat treatment includes: placing the high-temperature resistant multi-spectral compatible stealth material billet in a tube furnace and evacuating the furnace until the gas pressure inside the tube reaches 5×10⁻⁶. -4 Pa, under vacuum, was heated from room temperature to 800℃ at a heating rate of 4℃ / min and held at that temperature for 2 hours, and then cooled to room temperature at a cooling rate of 4℃ / min to obtain a high-temperature resistant multi-spectral compatible stealth material.

[0057] Example 4:

[0058] This embodiment provides a high-temperature resistant, multi-spectral compatible stealth material, including a substrate layer, a first functional layer, and a second functional layer. The first functional layer is located on the upper surface of the substrate layer, and the second functional layer is located on the upper surface of the first functional layer. The second functional layer is a titanium dioxide layer with uneven thickness, and the second functional layer includes three thickness modules with different thicknesses.

[0059] In this embodiment, the substrate is a nickel-based alloy substrate, specifically a K424 nickel-based high-temperature alloy substrate. This embodiment does not have a specific limitation on the source of the K424 nickel-based high-temperature alloy substrate; any commercially available alloy of the corresponding grade can be used. The first functional layer is a zirconium boride layer with uniform thickness, and the thickness of the first functional layer is 500 nm. In this embodiment, uniform thickness means that the thickness of each part of the first functional layer is consistent or slightly different, and the difference can be within 5 nm (for example, the thickness of the first functional layer falling within the range of 500 ± 5 nm is considered to be 500 nm).

[0060] In this embodiment, the three thickness modules of the second functional layer with different thicknesses are thickness module A (50nm), thickness module B (170nm), and thickness module C (200nm). Additionally, thicknesses within the range of 50±2nm are also classified as thickness module A, 170±2nm as thickness module B, and 200±2nm as thickness module C. In the visible light band, thickness module A appears blue, thickness module B appears green, and thickness module C appears yellow. The color can be adjusted appropriately according to the application environment to blend into the environment, achieving stealth in the visible light band, and further realizing multi-spectral stealth in the visible light-near-infrared-mid-far-infrared ranges.

[0061] In this embodiment, the number of thickness modules of any thickness in the second functional layer is at least one. When the number of thickness modules of any thickness in the second functional layer is not less than two, the thickness modules are randomly distributed or interleaved (for example, if the second functional layer includes three different thickness modules and the number of each thickness module is two, there are a total of six thickness modules, which are randomly distributed or interleaved). In this embodiment, the distribution of thickness modules of different thicknesses can be adjusted according to the actual application environment to ensure that the color rendering is similar to the environment, achieving the effect of blending into the environment and becoming invisible.

[0062] This embodiment also provides a method for preparing the high-temperature resistant, multi-spectral compatible stealth material of this embodiment, including the following steps:

[0063] S1. Pre-treat the substrate; specifically, the pre-treatment includes: cleaning the substrate with deionized water, then ultrasonically cleaning the substrate with anhydrous ethanol, and drying the substrate to obtain the pre-treated substrate.

[0064] S2. Sputter the first functional layer onto the pretreated substrate surface; the specific process is as follows: Place the pretreated substrate on a magnetron sputtering deposition stage; use a ZrB2 target with a diameter of 100 mm and a purity of 99.99% as the magnetron sputtering target, set the target-substrate distance to 500 nm, and set the sputtering distance to below 5 × 10⁻⁶ nm. -4Under a vacuum background of Pa, 99.99% pure argon gas was introduced into the sputtering chamber at a gas flow rate of 35 L / min until the sputtering pressure reached 2 Pa. Pre-sputtering was performed for 20 min at a sputtering power of 100 W and a sputtering rate of 50 nm / min. After pre-sputtering, sputtering was performed for 10 min at a sputtering rate of 50 nm / min under the conditions of sputtering power of 100 W, sputtering pressure of 0.9 Pa, and deposition temperature of room temperature to obtain a first functional layer with uniform thickness of 500 nm.

[0065] S3. Sputter a second functional layer onto the surface of the first functional layer to obtain a high-temperature resistant, multi-spectral compatible stealth material preform. The specific process is as follows: S31. Remove the substrate with the first functional layer sputtered from the sputtering cavity. According to the preset thickness module distribution of the second functional layer, use an organic film mold as a shielding mold to shield the thickness module B distribution area and the thickness module C distribution area. After shielding, place it on a magnetron sputtering deposition stage. S32. Use a Ti target with a diameter of 100 mm and a purity of 99.99% as the magnetron sputtering target. Set the target-substrate distance to 500 nm. The sputtering process is carried out at a temperature below 5 × 10⁻⁶ nm. -4 Under a vacuum background of Pa, argon gas with a purity of 99.99% and reactive gas O2 with a purity of 99.997% (volume ratio 12:1) are introduced into the sputtering chamber at a gas flow rate of 50 L / min until the sputtering pressure reaches 2 Pa. Sputtering is performed at a sputtering power of 80 W, a deposition temperature (substrate temperature) of 400 °C, and a sputtering rate of 50 nm / min. The deposition time is controlled until the sputtered thickness is the preset thickness of the unshielded thickness module minus the preset compensation thickness (e.g., the preset compensation thickness is 10 nm). S33: The sputtered product after S32 is removed from the sputtering chamber. The shielding mold on the low-thickness thickness module B distribution area in the unsputtered thickness module B distribution area and the thickness module C distribution area is removed. According to the preset thickness module distribution state of the second functional layer, the sputtering is performed... S34. The sputtered thickness module A and the unsputtered thickness module C distribution area are shielded by a shielding mold. After shielding, the material is placed on a magnetron sputtering deposition stage. S35. Repeat S36. After sputtering, the material is removed and the shielding mold on the unsputtered thickness module C distribution area is removed. According to the preset thickness module distribution state of the second functional layer, the sputtered thickness modules A and B are shielded by the shielding mold. After shielding, the material is placed on a magnetron sputtering deposition stage and S36 is repeated. S37. Remove all shielding molds and place the material on a magnetron sputtering deposition stage. Sputtering with preset compensation thickness is performed according to the sputtering parameters in step S36. After sputtering, a high-temperature multi-spectral compatible stealth material preform with non-mirror reflection and low infrared emissivity TiO2 / ZrB2 double layer film with three colors and infrared stealth characteristics is obtained.

[0066] S4. Heat treatment is performed on the high-temperature resistant multi-spectral compatible stealth material billet. The heat treatment includes: placing the high-temperature resistant multi-spectral compatible stealth material billet in a tube furnace and evacuating the furnace until the gas pressure inside the tube reaches 5×10⁻⁶. -4 Pa, under vacuum, was heated from room temperature to 820°C at a heating rate of 6°C / min and held at that temperature for 1 hour, and then cooled to room temperature at a cooling rate of 5°C / min to obtain a high-temperature resistant multi-spectral compatible stealth material.

[0067] The present invention conducted performance tests on the high-temperature resistant multi-spectral compatible stealth materials prepared in Examples 2-4, as detailed below:

[0068] (1) Infrared emissivity: Tested using an IR-2 dual-band emissivity meter.

[0069] For Example 2, in the 3-5 μm band, the infrared emissivity of the stealth material at 25℃, 150℃, and 300℃ is 0.203, 0.209, and 0.217, respectively; and in the 8-14 μm band, the infrared emissivity of the stealth material at 25℃, 150℃, and 300℃ is 0.082, 0.093, and 0.099, respectively. For Example 3, in the 3-5 μm band, the infrared emissivity of the stealth material at 25℃, 150℃, and 300℃ is 0.182, 0.195, and 0.213, respectively; and in the 8-14 μm band, the infrared emissivity of the stealth material at 25℃, 150℃, and 300℃ is 0.075, 0.082, and 0.097, respectively. For Example 4, in the 3-5μm band, the infrared emissivity of the stealth material at 25℃, 150℃, and 300℃ is 0.179, 0.182, and 0.193, respectively; and in the 8-14μm band, the infrared emissivity of the stealth material at 25℃, 150℃, and 300℃ is 0.071, 0.075, and 0.087, respectively.

[0070] (2) Impact resistance: Tested according to GB-T1732-1993 "Test Method for Impact Resistance of Coating Films"

[0071] For Example 2, the impact strength is 50 kg·cm; for Example 3, the impact strength is 55 kg·cm; and for Example 4, the impact strength is 62 kg·cm.

[0072] (3) Adhesion test: According to G81720-88 "Standard for Adhesion Rating of Coating Film", the adhesion level of the stealth materials in Examples 2-4 is all grade 1.

[0073] (4) Colorimetric parameter test: The test was conducted using an X·Rite QM200 portable colorimeter.

[0074] For Example 2, the total color difference ΔE of L*a*b* is 0.8; for Example 3, the total color difference ΔE of L*a*b* is 0.85; and for Example 4, the total color difference ΔE of L*a*b* is 0.88.

[0075] (5) High temperature resistance test: The test shall be conducted in accordance with GB / 1735-798 "Determination of heat resistance of paint film".

[0076] The stealth materials of Examples 2-4 were placed in an environment of 1000℃ for 60 hours. After 10 hours, 20 hours, 30 hours, 40 hours, 50 hours and 60 hours, the TiO2 / ZrB2 bilayer film was found to be intact and without cracking.

[0077] As can be seen, the stealth materials of Examples 2-4 of this invention have an infrared emissivity of approximately no more than 0.2 in the 3-5μm and 8-14μm bands, resulting in good infrared stealth performance; their impact resistance meets the requirements for use; the adhesion level of the film layers is all Grade 1, indicating good adhesion; the total color difference ΔE of L*a*b* is between 0.8 and 0.9, which can clearly distinguish color differences; they exhibit good color rendering in the visible light band and easily blend into the ambient color, achieving stealth in the visible light band; and the film layers remain intact and crack-free after long-term use in an environment of 1000℃, enabling high-temperature applications at 1000℃.

[0078] The present invention has been described above with reference to specific embodiments. These specific embodiments are merely exemplary and should not be construed as limiting the scope of protection of the present invention. Those skilled in the art can make various modifications, changes, or substitutions without departing from the essence of the present invention. Therefore, various equivalent variations made according to the present invention still fall within the scope of the present invention.

Claims

1. A high temperature resistant multi-spectrum compatible stealth material, characterized in that, The first functional layer is located on the upper surface of the substrate layer, and the second functional layer is located on the upper surface of the first functional layer. The second functional layer is a titanium dioxide layer with uneven thickness, and the second functional layer includes at least two thickness modules with different thicknesses. The substrate layer is a silicon wafer substrate or a nickel-based alloy substrate; the first functional layer is a zirconium boride layer with uniform thickness, and the thickness of the first functional layer is 300-500 nm. The specific process of obtaining the high-temperature-resistant multi-spectrum compatible stealth material blank is as follows: S31. The substrate with the first functional layer is taken out from the sputtering cavity, the high-thickness thickness module distribution area is shielded by the shielding mold according to the preset thickness module distribution state of the second functional layer, and the shielding mold is placed on the magnetron sputtering deposition platform after shielding. The volume ratio of argon to O2 is (5:1)-(12:1); the preset compensation thickness is 5-10 nm; S32, using the Ti target as a magnetron sputtering target, setting the target-substrate distance to be 100-500 mm, and introducing argon and a reaction gas O2 into the sputtering chamber at a flow rate of 20-50 L / min under a vacuum background of less than 5x10 -4 In the vacuum background of Pa, argon and reaction gas O2 are introduced into the sputtering chamber at a flow rate of 20-50 L / min until the sputtering pressure is 0.8-2 Pa, and sputtering is performed at a sputtering rate of 10-50 nm / min under the conditions of a sputtering power of 80-150 W and a deposition temperature of 280-400 ℃ until the sputtering thickness is the preset thickness of the unshielded thickness module minus the preset compensation thickness. S33. The product after sputtering in S32 is taken out from the sputtering cavity, the shielding mold on the low-thickness thickness module distribution area in the un-sputtered different-thickness thickness module distribution area is removed, the sputtered thickness module and the high-thickness thickness module distribution area in the un-sputtered different-thickness thickness module distribution area are shielded by the shielding mold according to the preset thickness module distribution state of the second functional layer, and the shielding mold is placed on the magnetron sputtering deposition platform after shielding. S34. Repeat the steps of S32 and S33 until all the preset thickness modules of the second functional layer are sputtered. S35. Remove all shielding molds and place them on the magnetron sputtering deposition platform. Sputter according to the sputtering parameters of step S32 to obtain a high-temperature-resistant multi-spectrum compatible stealth material blank. The thickness of the different-thickness thickness modules of the second functional layer is selected from 10-1000 nm. The number of any-thickness thickness modules of the second functional layer is at least one. When the number of any-thickness thickness modules of the second functional layer is not less than two, each thickness module is randomly distributed or spaced and staggered.

2. The high temperature resistant, multi-spectrum compatible stealth material of claim 1, wherein, The following steps are included:

3. The method of making a high temperature resistant, multi-spectrum compatible stealth material of any one of claims 1-2, wherein, S1. Pretreat the substrate; S2. Sputter the first functional layer on the upper surface of the pretreated substrate; S3. Sputter the second functional layer on the upper surface of the first functional layer to obtain a high-temperature-resistant multi-spectrum compatible stealth material blank; S4. Heat treat the high-temperature-resistant multi-spectrum compatible stealth material blank to obtain the high-temperature-resistant multi-spectrum compatible stealth material. The pretreatment includes: cleaning the substrate with deionized water, then ultrasonic cleaning the substrate with anhydrous ethanol, and drying to obtain the pretreated substrate.

4. The method of claim 3, wherein the high temperature resistant, multi-spectrum compatible stealth material is prepared by the steps of: The specific process of step S2 is as follows:

5. The method for preparing the high-temperature resistant multi-spectral compatible stealth material as described in claim 4, characterized in that, Place the pretreated substrate on the magnetron sputtering deposition platform; After the pre-sputtering is completed, sputter at a sputtering rate of 10-50 nm / min for 5-10 min under the conditions of a sputtering power of 100-400 W, a sputtering gas pressure of 0.2-0.9 Pa, and a deposition temperature of room temperature to obtain a first functional layer with uniform thickness. The ZrB2 target is used as a magnetron sputtering target, the target-substrate distance is set to 100-500mm, the sputtering gas pressure is set to 0.8-2Pa, the sputtering power is set to 100-400W, and the sputtering rate is set to 10-50nm / min. -4 The sputtering chamber is filled with argon at a flow rate of 25-35L / min under a vacuum background of 0.8-2Pa, and the sputtering power is set to 100-400W, and the sputtering rate is set to 10-50nm / min for 2-20min. The specific process of step S3 is as follows:

6. The method of claim 5, wherein the high temperature resistant, multi-spectrum compatible stealth material is prepared by the steps of: ​ S31, taking out the substrate sputtered with the first functional layer from the sputtering cavity, shielding the high-thickness thickness module distribution area according to the preset thickness module distribution state of the second functional layer by the shielding mold, and placing the shielding mold on the magnetron sputtering deposition stage after shielding; S32, using the Ti target as a magnetron sputtering target, setting the target-substrate distance to be 100-500 mm, and introducing argon and a reaction gas O2 into the sputtering chamber at a flow rate of 20-50 L / min under a vacuum background of less than 5x10 -4 In the vacuum background of Pa, argon and reaction gas O2 are introduced into the sputtering chamber at a flow rate of 20-50 L / min until the sputtering pressure is 0.8-2 Pa, and sputtering is performed at a sputtering rate of 10-50 nm / min under the conditions of a sputtering power of 80-150 W and a deposition temperature of 280-400 ℃ until the sputtering thickness is the preset thickness of the unshielded thickness module minus the preset compensation thickness. S33, taking out the product sputtered in S32 from the sputtering cavity, removing the shielding mold on the low-thickness thickness module distribution area in the un-sputtered different-thickness thickness module distribution area, shielding the sputtered thickness module and the high-thickness thickness module distribution area in the un-sputtered different-thickness thickness module distribution area according to the preset thickness module distribution state of the second functional layer by the shielding mold, and placing the shielding mold on the magnetron sputtering deposition stage after shielding; S34, repeating the steps of S32 and S33 until all the preset thickness modules of the second functional layer are sputtered completely; S35, removing all the shielding molds, placing them on the magnetron sputtering deposition stage, sputtering according to the sputtering parameters of the step S32 with a preset compensation thickness, and obtaining a high-temperature-resistant multi-spectrum compatible stealth material blank after sputtering.

7. The method for preparing the high-temperature resistant multi-spectral compatible stealth material as described in claim 6, characterized in that, The shielding mold is a metal mold or an organic film mold; in the step S32, the volume ratio of argon to O2 is (5:1)-(12:1); and the preset compensation thickness is 5-10 nm.

8. The method for preparing the high-temperature resistant multi-spectral compatible stealth material as described in claim 3, characterized in that, The heat treatment comprises: in a vacuum state, heating from room temperature to 760-820℃ at a heating rate of 2-6℃ / min, and then holding for 1-3h, and then cooling to room temperature at a cooling rate of 3-5℃ / min.