Antistatic intelligent thermal control coating and preparation method thereof
By designing a multi-layer film system and conductive paths on the spacecraft's thermal control coating, the problem of the intelligent thermal control coating not having anti-static properties was solved, adaptive regulation of infrared emissivity and electrostatic protection were achieved, and the space stability and safety of the spacecraft were improved.
Patent Information
- Application Number
- CN202510895570.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-30
- Publication Date
- 2025-09-19
AI Technical Summary
Existing intelligent thermal control coatings do not have anti-static properties, which may cause charging and discharging effects on spacecraft in the space environment, affecting the safety of the spacecraft and the normal operation of electronic equipment.
An antistatic intelligent thermal control coating is designed, consisting of a front film system and a back film system; the film system consists of a front reflective layer, a front dielectric layer, a front functional layer and a front conductive/protective layer; the back film system consists of a back conductive layer and a back protective layer; these layers are prepared on a substrate by magnetron sputtering, electron beam evaporation, pulsed laser deposition or atomic layer deposition methods to construct an asymmetric FP resonant cavity and a conductive path to achieve infrared emissivity regulation and electrostatic protection.
It realizes adaptive regulation of infrared emissivity at low and high temperatures, prevents charge accumulation on the spacecraft surface, improves the spatial stability and environmental adaptability of the coating, and is suitable for spacecraft thermal control systems affected by high-energy charged particles.
Smart Images
Figure CN120666293A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a thermal control coating and a preparation method thereof. Background Art
[0002] With the continuous development of major space missions such as manned space flight, lunar exploration, and deep space exploration, complex maneuvering and trajectory change missions have led spacecraft to encounter diverse thermal environments and space regions during operation. The reliability of the thermal control system directly determines the service life of the payload. Temperature-adaptive thermal control coatings are composite coating materials that passively control the emissivity of a spacecraft by varying its temperature, enabling autonomous regulation of the spacecraft's surface temperature. These coatings maintain the spacecraft's optimal operating temperature and offer advantages such as lightweight, energy-efficient, and high reliability. However, thermal control coatings covering the outer surface of a spacecraft are often exposed to the harsh environment of space, requiring them to possess not only excellent thermal control performance but also good adaptability to the space environment. As a representative thermochromic material, VO2 has attracted widespread attention and is being increasingly applied in the field of intelligent thermal control due to its significant changes in infrared optical properties before and after the metal-insulator phase transition. Furthermore, by constructing an asymmetric FP resonant cavity, multi-beam interference can be achieved, enhancing the high-temperature infrared absorptivity of the structure and further improving the control performance of VO2-based intelligent thermal control coatings. However, VO2 is in an insulating state at low temperatures. This influence can lead to severe charge-discharge effects on the coating surface during in-orbit use due to the influence of high-energy charged particles in space. When the accumulated charge on the satellite surface exceeds the breakdown threshold, discharge occurs, posing a serious threat to spacecraft safety. The resulting electric field can not only damage the intelligent thermal control components themselves but also interfere with the normal operation of electronic equipment. Therefore, the development of new anti-static intelligent thermal control coatings is urgently needed. Summary of the Invention
[0003] The present invention aims to solve the problem that existing intelligent thermal control coatings do not have antistatic properties, and further provides an antistatic intelligent thermal control coating and a preparation method thereof.
[0004] An antistatic intelligent thermal control coating, which consists of a substrate, a front film system and a back film system;
[0005] The front film system is composed of a front reflective layer, a front dielectric layer, a front functional layer and a front conductive / protective layer; the back film system is composed of a back conductive layer and a back protective layer;
[0006] The front surface of the substrate is composed of a front reflective layer, a front dielectric layer, a front functional layer and a front conductive / protective layer in order from the surface of one side of the substrate upward;
[0007] The back side of the base is sequentially provided with a reverse conductive layer and a reverse protective layer from the other side surface of the base downwards.
[0008] A method for preparing an antistatic intelligent thermal control coating is carried out according to the following steps:
[0009] 1. Substrate cleaning:
[0010] cleaning and drying the substrate to obtain a pretreated substrate;
[0011] 2. Preparation of the front film system:
[0012] Using magnetron sputtering, electron beam evaporation, pulsed laser deposition or atomic layer deposition, a front reflective layer, a front dielectric layer, a front functional layer and a front conductive / protective layer are sequentially prepared on one surface of the pretreated substrate to obtain a substrate covered with a front film system;
[0013] 3. Preparation of reverse film system:
[0014] By using magnetron sputtering, electron beam evaporation, pulsed laser deposition or atomic layer deposition, a reverse conductive layer and a reverse protective layer are sequentially prepared on the other surface of the substrate covered with the front film system to obtain an antistatic intelligent thermal control coating.
[0015] The beneficial effects of the present invention are:
[0016] Based on the requirements of spacecraft thermal control coatings for light weight, energy saving and high space stability, the present invention provides an antistatic intelligent thermal control coating and a preparation method thereof, which has the advantages of large emissivity control range, good cycle stability, light weight, passive control, good electrostatic protection stability, etc.; the antistatic intelligent thermal control coating has a low infrared emissivity of 0.12~0.30 under low temperature conditions and a high infrared emissivity of 0.60~0.77 under high temperature conditions, and can realize adaptive temperature control of emissivity to ensure that the spacecraft is in a safe operating temperature range. At the same time, the front and back resistance is lower than 100kΩ, which can effectively prevent the accumulation of surface charge on the spacecraft, has excellent electrostatic protection performance, and is very suitable for spacecraft thermal control systems in service orbits with large changes in external heat flux density and the influence of high-energy charged particles.
[0017] (1) The use of a front reflective layer, a front dielectric layer and a front functional layer to construct an asymmetric FP resonant cavity can significantly and effectively improve the infrared emissivity modulation amplitude of the intelligent thermal control coating. By changing the thickness of the front dielectric layer and the front functional layer, the high and low temperature infrared emissivity can be precisely controlled to meet the low temperature insulation and high temperature heat dissipation requirements of different spacecraft. Compared with traditional intelligent thermal control coatings and active control intelligent thermal control coatings, it effectively avoids the direct impact of heat flow changes outside space on the spacecraft and the additional energy consumption.
[0018] (2) By doping elements, the phase transition temperature of the front functional layer can be changed, and the operating temperature range of the intelligent thermal control coating can be further changed to adapt to the use requirements of different spacecraft.
[0019] (3) The conductive path is constructed through the combined action of the front and back conductive layers, which effectively reduces the resistance of the front and back surfaces of the coating, prevents the accumulation of charge on the coating surface, and improves the spatial stability of the intelligent thermal control coating.
[0020] (4) The introduction of a reverse protective layer with high oxidation resistance can effectively isolate oxygen and water vapor, preventing the back metal conductive layer from being oxidized and causing an increase in resistivity when placed in a hot and humid atmospheric environment for a long time, making the device have excellent environmental stability.
[0021] (5) The prepared thin film materials can be obtained by a variety of preparation methods, such as magnetron sputtering, electron beam evaporation, pulsed laser deposition and atomic layer deposition, etc., with a variety of preparation processes, simple methods, low cost, high repeatability and large-scale preparation. In terms of process implementation and engineering application, they can be mass-produced and have high reliability. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] Figure 1 Schematic diagram of the structure of the antistatic intelligent thermal control coating of the present invention, 1 is the substrate, 2 is the front reflective layer, 3 is the front dielectric layer, 4 is the front functional layer, 5 is the front conductive / protective layer, 6 is the back conductive layer, and 7 is the back protective layer;
[0023] Figure 2 This is a temperature-dependent reflectance spectrum of the antistatic intelligent thermal control coating prepared in Example 1 in the 2.5μm~25μm band. DETAILED DESCRIPTION
[0024] Specific implementation method 1, combined with Figure 1 Specific description: This embodiment is an antistatic intelligent thermal control coating, which consists of a substrate, a front film system and a back film system;
[0025] The front film system is composed of a front reflective layer, a front dielectric layer, a front functional layer and a front conductive / protective layer; the back film system is composed of a back conductive layer and a back protective layer;
[0026] The front surface of the substrate is composed of a front reflective layer, a front dielectric layer, a front functional layer and a front conductive / protective layer in order from the surface of one side of the substrate upward;
[0027] The back side of the base is sequentially provided with a reverse conductive layer and a reverse protective layer from the other side surface of the base downwards.
[0028] In this embodiment, the substrate may be any rigid or flexible substrate with a flat and smooth surface.
[0029] In this specific embodiment, the front reflective layer may be made of other materials with a reflectivity of more than 80% in the infrared band.
[0030] In this specific embodiment, the front dielectric layer may be a lossless dielectric layer material having a relatively low refractive index in the infrared band of 2.5 μm to 25 μm.
[0031] In this specific embodiment, when the temperature of the front functional layer is lower than the phase transition temperature, the thermal control coating exhibits low infrared emissivity, and when the temperature is higher than the phase transition temperature, the thermal control coating exhibits high infrared emissivity; the device operating temperature range can be adjusted by doping with different elements and adjusting the element doping amount.
[0032] The thicknesses of the front dielectric layer and the front functional layer described in this specific embodiment can be coupled and adjusted to obtain different emissivities to meet the usage requirements of different spacecraft.
[0033] In this specific embodiment, the front conductive / protective layer and the back conductive layer work together to make the device's front and back resistance ≤200kΩ, preventing charge accumulation on the thermal control coating surface caused by high-energy charged particle irradiation. At the same time, as a protective layer, it can prevent surface oxidation of the front functional layer caused by long-term exposure to the atmospheric environment, further improving the environmental stability of the coating. The front conductive / protective layer can be replaced with a transparent conductive oxide with high transmittance and low resistivity in the infrared band;
[0034] In this embodiment, the reverse conductive layer may be made of a conductive oxide having a sheet resistance lower than 50Ω / sq;
[0035] In this specific embodiment, the reverse protective layer prevents the reverse conductive layer from being oxidized, and may also be replaced with other high-performance materials such as Cu alloy and iron-chromium-aluminum alloy with high conductivity and oxidation resistance.
[0036] The beneficial effects of this embodiment are:
[0037] Based on the requirements of spacecraft thermal control coatings for light weight, energy saving and high space stability, this embodiment provides an antistatic intelligent thermal control coating and a preparation method thereof, which has the advantages of large emissivity control range, good cycle stability, light weight, passive control, and good electrostatic protection stability; the antistatic intelligent thermal control coating has a low infrared emissivity of 0.12~0.30 under low temperature conditions and a high infrared emissivity of 0.60~0.77 under high temperature conditions, and can realize adaptive temperature control of emissivity to ensure that the spacecraft is in a safe operating temperature range. At the same time, the front and back resistance is less than 100kΩ, which can effectively prevent the accumulation of charge on the spacecraft surface, and has excellent electrostatic protection performance. It is very suitable for spacecraft thermal control systems in service orbits with large changes in external heat flux density and the influence of high-energy charged particles.
[0038] (1) The use of a front reflective layer, a front dielectric layer and a front functional layer to construct an asymmetric FP resonant cavity can significantly and effectively improve the infrared emissivity modulation amplitude of the intelligent thermal control coating. By changing the thickness of the front dielectric layer and the front functional layer, the high and low temperature infrared emissivity can be precisely controlled to meet the low temperature insulation and high temperature heat dissipation requirements of different spacecraft. Compared with traditional intelligent thermal control coatings and active control intelligent thermal control coatings, it effectively avoids the direct impact of heat flow changes outside space on the spacecraft and the additional energy consumption.
[0039] (2) By doping elements, the phase transition temperature of the front functional layer can be changed, and the operating temperature range of the intelligent thermal control coating can be further changed to adapt to the use requirements of different spacecraft.
[0040] (3) The conductive path is constructed through the combined action of the front and back conductive layers, which effectively reduces the resistance of the front and back surfaces of the coating, prevents the accumulation of charge on the coating surface, and improves the spatial stability of the intelligent thermal control coating.
[0041] (4) The introduction of a reverse protective layer with high oxidation resistance can effectively isolate oxygen and water vapor, preventing the back metal conductive layer from being oxidized and causing an increase in resistivity when placed in a hot and humid atmospheric environment for a long time, making the device have excellent environmental stability.
[0042] (5) The prepared thin film materials can be obtained by a variety of preparation methods, such as magnetron sputtering, electron beam evaporation, pulsed laser deposition and atomic layer deposition, etc., with a variety of preparation processes, simple methods, low cost, high repeatability and large-scale preparation. In terms of process implementation and engineering application, they can be mass-produced and have high reliability.
[0043] Specific embodiment 2: This embodiment differs from specific embodiment 1 in that the substrate is made of quartz glass, sapphire substrate, aluminum sheet, silicon wafer or zirconia ceramic, and has a thickness of 0.1 mm to 1 mm. Other aspects are the same as specific embodiment 1.
[0044] Specific embodiment 3: This embodiment differs from specific embodiment 1 or 2 in that the front reflective layer is made of Al, Au, Ag, Cu, W, TiN, ITO, or AZO, and has a thickness of 150 nm to 250 nm. Other aspects are the same as specific embodiment 1 or 2.
[0045] Specific embodiment 4: This embodiment differs from specific embodiments 1 to 3 in that the front dielectric layer is made of HfO2, CaF2, SiO2, ZnO, TiO2, MgF2, Al2O3, or ZrO2, and has a thickness of 500nm to 1000nm. Other aspects are the same as specific embodiments 1 to 3.
[0046] Specific embodiment 5: This embodiment differs from specific embodiments 1 to 4 in that the front functional layer is VO2 or element-doped VO2, and has a thickness of 30nm to 100nm. It is the same as specific embodiments 1 to 4.
[0047] Specific embodiment 6: This embodiment differs from specific embodiments 1 to 5 in that the front conductive / protective layer is made of ITO, AZO or GZO and has a thickness of 50 nm to 100 nm. Other aspects are the same as specific embodiments 1 to 5.
[0048] Specific embodiment 7: This embodiment differs from specific embodiments 1 to 6 in that the reverse conductive layer is made of Al, Au, Ag, Cu, ITO, AZO, GZO, or FTO, and has a thickness of 100 nm to 200 nm. Other aspects are the same as specific embodiments 1 to 6.
[0049] Specific embodiment 8: This embodiment differs from specific embodiments 1 to 7 in that the reverse side protective layer is made of nickel-chromium alloy, Cu alloy or iron-chromium-aluminum alloy and has a thickness of 100 nm to 200 nm. Other aspects are the same as specific embodiments 1 to 7.
[0050] Specific embodiment 9: This embodiment provides a method for preparing an antistatic intelligent thermal control coating, which is carried out according to the following steps:
[0051] 1. Substrate cleaning:
[0052] cleaning and drying the substrate to obtain a pretreated substrate;
[0053] 2. Preparation of the front film system:
[0054] Using magnetron sputtering, electron beam evaporation, pulsed laser deposition or atomic layer deposition, a front reflective layer, a front dielectric layer, a front functional layer and a front conductive / protective layer are sequentially prepared on one surface of the pretreated substrate to obtain a substrate covered with a front film system;
[0055] 3. Preparation of reverse film system:
[0056] By using magnetron sputtering, electron beam evaporation, pulsed laser deposition or atomic layer deposition, a reverse conductive layer and a reverse protective layer are sequentially prepared on the other surface of the substrate covered with the front film system to obtain an antistatic intelligent thermal control coating.
[0057] Specific embodiment 10: This embodiment differs from specific embodiment 9 in that the preparation of the front film system in step 2 is specifically carried out according to the following steps:
[0058] ① When the vacuum degree is lower than 1×10 -3Under the conditions of 0.4 Pa to 1.0 Pa, an argon gas flow rate of 70 sccm to 100 sccm, a substrate temperature of room temperature to 200° C., and a DC power of 100 W to 200 W, a front reflective layer is obtained on one side of the pretreated substrate by DC magnetron sputtering;
[0059] ② When the vacuum degree is lower than 1.5×10 -3 Under the conditions of 0.4 Pa to 1.0 Pa, an argon gas flow rate of 70 sccm to 100 sccm, a substrate temperature of 200°C to 400°C, and a DC power of 100 W to 250 W, a front dielectric layer is formed on the surface of the front reflective layer by DC magnetron sputtering;
[0060] ③ When the vacuum degree is lower than 1.2×10 -3 Under the conditions of 1.5-2.0 Pa, 1.5-2.0 frequency, 350 Hz-400 Hz pulse width, 45 μs-50 μs power, 180 W-200 W high-power pulse voltage, 450 V-510 V high-pressure, 0.4 Pa-1.2 Pa, argon flow rate of 80 sccm-85 sccm, oxygen flow rate of 0.8 sccm-2.2 sccm and substrate temperature of 180°C-400°C, high-power pulse magnetron sputtering is performed on the surface of the front dielectric layer, and then the temperature is increased to 300°C-400°C under the conditions of argon flow rate of 60 sccm-120 sccm and heating rate of 1°C / min-5°C / min, and kept warm for 1 h-6 h under the conditions of argon flow rate of 60 sccm-120 sccm and temperature of 300°C-400°C, and finally naturally cooled to room temperature to obtain the front functional layer;
[0061] ④ When the vacuum degree is lower than 2.0×10 -3 Under the conditions of 1.0 Pa, 350 Hz to 400 Hz frequency, 45 μs to 50 μs pulse width, 100 W to 200 W power, 500 V to 550 V high-power pulse voltage, 0.4 Pa to 1.0 Pa pressure, 70 sccm to 90 sccm argon flow rate, 0 sccm to 5 sccm oxygen flow rate, and 50° C. to 400° C. substrate temperature, a front conductive / protective layer is obtained on the surface of the front functional layer by high-power pulse magnetron sputtering, thereby obtaining a substrate covered with a front film system;
[0062] Or when the vacuum degree is lower than 2.0×10 -3 Under the conditions of 100W~250W RF power, 0.4Pa~1.2Pa, 60sccm~120sccm argon flow rate and 50℃~400℃ substrate temperature, a front conductive / protective layer is formed on the surface of the front functional layer by RF magnetron sputtering to obtain a substrate covered with a front film system;
[0063] The preparation of the reverse film system in step 3 is specifically carried out according to the following steps:
[0064] ① When the vacuum degree is lower than 1×10 -3 Under the conditions of 0.4 Pa to 1.0 Pa, an argon gas flow rate of 70 sccm to 100 sccm, a substrate temperature of room temperature to 200°C, and a DC power of 100 W to 200 W, a reverse conductive layer is obtained by DC magnetron sputtering on the surface of the other side of the substrate covered with the front film system;
[0065] ② When the vacuum degree is lower than 1.8×10 -3 Under the following conditions: 1.5 Pa, 0.4 Pa to 1.2 Pa, argon gas flow rate of 70 sccm to 100 sccm, substrate temperature of room temperature to 200°C, and DC power of 100 W to 200 W, a reverse protective layer is formed on the reverse conductive layer by DC magnetron sputtering, thereby obtaining an antistatic intelligent thermal control coating. Other aspects are the same as those of the ninth embodiment.
[0066] The following examples are used to verify the beneficial effects of the present invention:
[0067] Example 1:
[0068] An antistatic intelligent thermal control coating, which consists of a substrate, a front film system and a back film system;
[0069] The front film system is composed of a front reflective layer, a front dielectric layer, a front functional layer and a front conductive / protective layer; the back film system is composed of a back conductive layer and a back protective layer;
[0070] The front surface of the substrate is composed of a front reflective layer, a front dielectric layer, a front functional layer and a front conductive / protective layer in order from the surface of one side of the substrate upward;
[0071] The back side of the base is sequentially provided with a reverse conductive layer and a reverse protective layer from the other side surface of the base downwards.
[0072] The substrate is made of quartz glass and has a thickness of 0.2 mm.
[0073] The front reflective layer is Al, has an infrared reflectivity of 92%, and a thickness of 150 nm.
[0074] The front dielectric layer is HfO2 and has a thickness of 600nm.
[0075] The front functional layer is W-doped VO2, where W accounts for 2% of the total number of W and V atoms and has a thickness of 50 nm.
[0076] The front conductive / protective layer is ITO with a thickness of 50 nm.
[0077] The reverse conductive layer is Al and has a thickness of 100 nm.
[0078] The reverse protective layer is a Ni-Cr alloy, wherein the mass percentage of Ni in the Ni-Cr alloy is 80%, the mass percentage of Cr is 20%, and the thickness is 100 nm.
[0079] The above-mentioned method for preparing an antistatic intelligent thermal control coating is carried out according to the following steps:
[0080] 1. Substrate cleaning:
[0081] The substrate was ultrasonically cleaned with acetone, anhydrous ethanol, and deionized water in sequence, and then dried at 80°C for 6 hours to obtain a pretreated substrate.
[0082] 2. Preparation of the front reflective layer:
[0083] Using metal Al target, the vacuum degree is 8×10 -4 Under the conditions of 0.8 Pa, working gas pressure of 0.8 Pa, argon flow rate of 90 sccm, substrate temperature of 200°C and DC power of 150 W, a front reflective layer was obtained on the surface of one side of the pretreated substrate by DC magnetron sputtering;
[0084] 3. Preparation of the front dielectric layer:
[0085] Using a metal Hf target, the vacuum degree was 1.0×10 -3 The front dielectric layer was formed on the surface of the front reflective layer by DC magnetron sputtering under the conditions of 0.8 Pa, working gas pressure of 0.8 Pa, argon flow rate of 80 sccm, substrate temperature of 200°C and DC power of 180 W.
[0086] 4. Preparation of the front functional layer:
[0087] Using WV target, the vacuum degree is 1.0×10 -3 Pa, frequency 400 Hz, pulse width 50 μs, power 180 W, high-power pulse voltage 510 V, pressure 0.8 Pa, argon flow rate 80 sccm, oxygen flow rate 1.2 sccm and substrate temperature 200 ° C, high-power pulse magnetron sputtering was performed on the surface of the front dielectric layer, and then the temperature was increased to 400 ° C under the conditions of argon flow rate 100 sccm and heating rate 1 ° C / min, and kept at 400 ° C for 5 hours under the conditions of argon flow rate 100 sccm and temperature, and finally naturally cooled to room temperature to obtain the front functional layer;
[0088] 5. Preparation of the front conductive / protective layer:
[0089] Using ITO target, the vacuum degree is 1.5×10 -3Under the conditions of 100 Pa, 400 Hz frequency, 50 μs pulse width, 180 W power, 530 V high-power pulse voltage, 0.8 Pa pressure, 80 sccm argon flow rate, 4.2 sccm oxygen flow rate and 200°C substrate temperature, high-power pulse magnetron sputtering was performed on the surface of the front functional layer to obtain a front conductive / protective layer, thereby obtaining a substrate covered with a front film system;
[0090] 6. Preparation of the reverse conductive layer:
[0091] Using metal Al target, the vacuum degree is 8×10 -4 Under the conditions of 0.8 Pa, working gas pressure of 0.8 Pa, argon flow rate of 90 sccm, substrate temperature of 200°C and DC power of 150 W, a reverse conductive layer was obtained by DC magnetron sputtering on the surface of the other side of the substrate covered with the front film system;
[0092] 7. Preparation of the reverse protective layer:
[0093] Using nickel-chromium alloy targets, the vacuum degree is 1.5×10 -3 Under the conditions of 0.05 Pa, working gas pressure of 1.0 Pa, argon flow rate of 80 sccm, substrate temperature of 200 ° C and DC power of 200 W, DC magnetron sputtering was performed on the surface of the reverse conductive layer to obtain a reverse protective layer, that is, an antistatic intelligent thermal control coating.
[0094] In this embodiment, a Fourier transform infrared spectrometer is used to test the hemispherical infrared emissivity of the antistatic intelligent thermal control coating. The low-temperature emissivity and high-temperature emissivity of the sample are tested. If the infrared emissivity of the sample meets the spacecraft thermal control requirements, the sample can be saved and the preparation is completed. Otherwise, it needs to be re-prepared.
[0095] This example uses a high-precision multimeter to test the front and back resistance of the antistatic intelligent thermal control coating. If the test resistance meets the requirements, the sample can be saved and the preparation is complete. Otherwise, it needs to be re-prepared. The front and back resistance is the resistance from the front to the back of the test sample. Specifically, the back of the sample is placed on a conductive substrate. Use one probe of the multimeter to touch the front of the sample and the other probe to touch the conductive substrate.
[0096] Figure 2 This figure shows the temperature-dependent reflectance spectrum of the antistatic intelligent thermal control coating prepared in Example 1 in the 2.5μm-25μm wavelength range. The coating's infrared emissivity was calculated to be 0.19 at 0°C and 0.65 at 70°C. The antistatic intelligent thermal control coating exhibits high reflectivity at low temperatures and low reflectivity at high temperatures. The reflectance spectra of the intelligent thermal control coating before and after the VO2 phase transition differ significantly, demonstrating excellent emissivity control capabilities.
[0097] The antistatic intelligent thermal control coating prepared in Example 1 was tested for infrared reflectance spectroscopy over a wavelength range of 2.5 μm to 25 μm. The calculated phase transition temperature was 27°C, the infrared emissivity was 0.19 at 0°C, and 0.65 at 70°C. The surface resistance was 8.0 kΩ.
[0098] Example 2: This example differs from Example 1 in that the thickness of the front dielectric layer is 700 nm. Other aspects are the same as Example 1.
[0099] The antistatic intelligent thermal control coating prepared in Example 2 was tested for infrared reflectance spectroscopy at varying temperatures over a wavelength range of 2.5 μm to 25 μm. The calculated phase transition temperature was 27°C, the infrared emissivity was 0.21 at 0°C, and 0.64 at 70°C, with a front-to-back resistivity of 8.8 kΩ.
[0100] Example 3: This example differs from Example 1 in that the thickness of the front dielectric layer is 800 nm, and the thickness of the front functional layer is 40 nm. Other aspects are the same as Example 1.
[0101] The antistatic intelligent thermal control coating prepared in Example 3 was tested for infrared reflectance spectroscopy at varying temperatures over a wavelength range of 2.5 μm to 25 μm. The calculated phase transition temperature was 27°C, the infrared emissivity was 0.24 at 0°C, and 0.68 at 70°C, with a front and back surface resistance of 15.5 kΩ.
[0102] Example 4: This example differs from Example 1 in that the thickness of the front dielectric layer is 900 nm, and the thickness of the front functional layer is 40 nm. Other aspects are the same as Example 1.
[0103] The antistatic intelligent thermal control coating prepared in Example 4 was tested for infrared reflectance spectroscopy over a wavelength range of 2.5 μm to 25 μm. The calculated phase transition temperature was 27°C, the infrared emissivity was 0.26 at 0°C, and 0.71 at 70°C. The resistivity on both sides was 30.4 kΩ.
[0104] Example 5: This example differs from Example 1 in that the thickness of the front dielectric layer is 900 nm, and the thickness of the front functional layer is 60 nm. Other aspects are the same as Example 1.
[0105] The antistatic intelligent thermal control coating prepared in Example 5 was tested for infrared reflectance spectroscopy at varying temperatures over a wavelength range of 2.5 μm to 25 μm. The calculated phase transition temperature was 27°C, the infrared emissivity was 0.30 at 0°C, and 0.77 at 70°C, with a front-to-back resistivity of 55.7 kΩ.
[0106] Example 6: This example differs from Example 1 in that the material of the front functional layer is VO2. Other aspects are the same as Example 1.
[0107] The antistatic intelligent thermal control coating prepared in Example 6 was tested for variable-temperature infrared reflectance spectroscopy over a wavelength range of 2.5 μm to 25 μm. The calculated phase transition temperature was 67.5°C, the infrared emissivity was 0.20 at 20°C, and 0.65 at 100°C, with a front-to-back resistivity of 41.1 kΩ.
[0108] Example 7: This example differs from Example 1 in that the W-doped VO2 accounts for 1.5% of the total number of W and V atoms. Other aspects are the same as Example 1.
[0109] The antistatic intelligent thermal control coating prepared in Example 7 was tested for infrared reflectance spectroscopy at varying temperatures over a wavelength range of 2.5 μm to 25 μm. The calculated phase transition temperature was 38°C, the infrared emissivity was 0.20 at 0°C, and 0.64 at 100°C, with a front-to-back resistivity of 20.7 kΩ.
[0110] Example 8: This example differs from Example 1 in that the W-doped VO2 accounts for 2.5% of the total number of W and V atoms. Other aspects are the same as Example 1.
[0111] The antistatic intelligent thermal control coating prepared in Example 8 was tested for infrared reflectance spectroscopy over a wavelength range of 2.5 μm to 25 μm. The calculated phase transition temperature was 17.5°C, the infrared emissivity was 0.17 at -20°C, and 0.64 at 70°C. The surface resistance was 6.5 kΩ.
[0112] Example 9: This example differs from Example 1 in that W in the W-doped VO2 accounts for 3% of the total number of W and V atoms. Other aspects are the same as Example 1.
[0113] The antistatic intelligent thermal control coating prepared in Example 9 was tested for infrared reflectance spectroscopy over a wavelength range of 2.5 μm to 25 μm. The calculated phase transition temperature was 7°C, the infrared emissivity was 0.12 at -20°C, and 0.60 at 40°C, with a front and back surface resistance of 3.3 kΩ.
[0114] Example 10: This example differs from Example 1 in that: in step 5, an ITO target is used and the vacuum degree is 1.5×10 -3Under the conditions of 0.5 Pa, RF power of 150 W, pressure of 0.9 Pa, argon flow rate of 100 sccm, and substrate temperature of 200°C, RF magnetron sputtering was performed on the surface of the front functional layer to form a front conductive / protective layer, thereby obtaining a substrate covered with a front film system. Other aspects were the same as in Example 1.
[0115] The antistatic intelligent thermal control coating prepared in Example 10 was tested for infrared reflectance spectroscopy at varying temperatures over a wavelength range of 2.5 μm to 25 μm. The calculated phase transition temperature was 27°C, the infrared emissivity was 0.24 at 0°C, and 0.65 at 70°C, with a front and back surface resistance of 4.9 kΩ.
[0116] Comparative Experiment 1: This comparative experiment differs from Example 1 in that the front conductive / protective layer is omitted. Other aspects are the same as Example 1.
[0117] The antistatic intelligent thermal control coating prepared in Comparative Experiment 1 was tested by infrared reflectance spectroscopy at varying temperatures over a wavelength range of 2.5 μm to 25 μm. The calculated phase transition temperature was 27°C, the infrared emissivity was 0.18 at 0°C, and 0.65 at 70°C. The resistivity on both sides was 9.9 MΩ.
[0118] Comparative Experiment 2: This comparative experiment differs from Example 1 in that the reverse film system is omitted. Other aspects are the same as Example 1.
[0119] The antistatic intelligent thermal control coating prepared in Comparative Experiment 2 was tested with infrared reflectance spectroscopy over a wavelength range of 2.5μm to 25μm. The calculated phase transition temperature was 27°C, the infrared emissivity was 0.19 at 0°C, and 0.65 at 70°C. There was no conductive path between the front and back sides of the sample, and the resistance between the front and back sides was ∞.
Claims
1. An antistatic intelligent thermal control coating, characterized in that It consists of a base, a front film system and a back film system; The front film system is composed of a front reflective layer, a front dielectric layer, a front functional layer and a front conductive / protective layer; the back film system is composed of a back conductive layer and a back protective layer; The front surface of the substrate is composed of a front reflective layer, a front dielectric layer, a front functional layer and a front conductive / protective layer in order from the surface of one side of the substrate upward; The back side of the base is sequentially provided with a reverse conductive layer and a reverse protective layer from the other side surface of the base downwards.
2. The antistatic intelligent thermal control coating according to claim 1, characterized in that The substrate is quartz glass, sapphire substrate, metal aluminum sheet, silicon sheet or zirconia ceramic, and has a thickness of 0.1mm to 1mm.
3. The antistatic intelligent thermal control coating according to claim 1, characterized in that The front reflective layer is made of Al, Au, Ag, Cu, W, TiN, ITO or AZO, and has a thickness of 150nm to 250nm.
4. The antistatic intelligent thermal control coating according to claim 1, characterized in that The front dielectric layer is made of HfO2, CaF2, SiO2, ZnO, TiO2, MgF2, Al2O3 or ZrO2, and has a thickness of 500nm~1000nm.
5. The antistatic intelligent thermal control coating according to claim 1, characterized in that The front functional layer is VO2 or element-doped VO2, and has a thickness of 30nm~100nm.
6. The antistatic intelligent thermal control coating according to claim 1, characterized in that The front conductive / protective layer is made of ITO, AZO or GZO, and has a thickness of 50nm to 100nm.
7. The antistatic intelligent thermal control coating according to claim 1, characterized in that The reverse conductive layer is made of Al, Au, Ag, Cu, ITO, AZO, GZO or FTO, and has a thickness of 100nm to 200nm.
8. The antistatic intelligent thermal control coating according to claim 1, characterized in that The reverse side protection layer is made of nickel-chromium alloy, Cu alloy or iron-chromium-aluminum alloy, and has a thickness of 100nm-200nm.
9. The method for preparing an antistatic intelligent thermal control coating according to claim 1, characterized in that It is carried out in the following steps:
1. Substrate cleaning: cleaning and drying the substrate to obtain a pretreated substrate; 2. Preparation of the front film system: Using magnetron sputtering, electron beam evaporation, pulsed laser deposition or atomic layer deposition, a front reflective layer, a front dielectric layer, a front functional layer and a front conductive / protective layer are sequentially prepared on one surface of the pretreated substrate to obtain a substrate covered with a front film system; 3. Preparation of reverse film system: By using magnetron sputtering, electron beam evaporation, pulsed laser deposition or atomic layer deposition, a reverse conductive layer and a reverse protective layer are sequentially prepared on the other surface of the substrate covered with the front film system to obtain an antistatic intelligent thermal control coating.
10. The method for preparing an antistatic intelligent thermal control coating according to claim 9, characterized in that The preparation of the front film system in step 2 is specifically carried out according to the following steps: ① When the vacuum degree is lower than 1×10 -3 Under the conditions of 0.4 Pa to 1.0 Pa, an argon gas flow rate of 70 sccm to 100 sccm, a substrate temperature of room temperature to 200° C., and a DC power of 100 W to 200 W, a front reflective layer is obtained on one side of the pretreated substrate by DC magnetron sputtering; ② When the vacuum degree is lower than 1.5×10 -3 Under the conditions of 0.4 Pa to 1.0 Pa, an argon gas flow rate of 70 sccm to 100 sccm, a substrate temperature of 200°C to 400°C, and a DC power of 100 W to 250 W, a front dielectric layer is formed on the surface of the front reflective layer by DC magnetron sputtering; ③ When the vacuum degree is lower than 1.2×10 -3 Under the conditions of 1.5-2.0 Pa, 1.5-2.0 frequency, 350 Hz-400 Hz pulse width, 45 μs-50 μs power, 180 W-200 W high-power pulse voltage, 450 V-510 V high-pressure, 0.4 Pa-1.2 Pa, argon flow rate of 80 sccm-85 sccm, oxygen flow rate of 0.8 sccm-2.2 sccm and substrate temperature of 180°C-400°C, high-power pulse magnetron sputtering is performed on the surface of the front dielectric layer, and then the temperature is increased to 300°C-400°C under the conditions of argon flow rate of 60 sccm-120 sccm and heating rate of 1°C / min-5°C / min, and kept warm for 1 h-6 h under the conditions of argon flow rate of 60 sccm-120 sccm and temperature of 300°C-400°C, and finally naturally cooled to room temperature to obtain the front functional layer; ④ When the vacuum degree is lower than 2.0×10 -3 Under the conditions of 1.0 Pa, 350 Hz to 400 Hz frequency, 45 μs to 50 μs pulse width, 100 W to 200 W power, 500 V to 550 V high-power pulse voltage, 0.4 Pa to 1.0 Pa pressure, 70 sccm to 90 sccm argon flow rate, 0 sccm to 5 sccm oxygen flow rate, and 50° C. to 400° C. substrate temperature, a front conductive / protective layer is obtained on the surface of the front functional layer by high-power pulse magnetron sputtering, thereby obtaining a substrate covered with a front film system; Or when the vacuum degree is lower than 2.0×10 -3 Under the conditions of 100W~250W RF power, 0.4Pa~1.2Pa, 60sccm~120sccm argon flow rate and 50℃~400℃ substrate temperature, a front conductive / protective layer is formed on the surface of the front functional layer by RF magnetron sputtering to obtain a substrate covered with a front film system; The preparation of the reverse film system in step 3 is specifically carried out according to the following steps: ① When the vacuum degree is lower than 1×10 -3 Under the conditions of 0.4 Pa to 1.0 Pa, an argon gas flow rate of 70 sccm to 100 sccm, a substrate temperature of room temperature to 200°C, and a DC power of 100 W to 200 W, a reverse conductive layer is obtained by DC magnetron sputtering on the surface of the other side of the substrate covered with the front film system; ② When the vacuum degree is lower than 1.8×10 -3 Under the conditions of 0.4 Pa ~ 1.2 Pa, working gas pressure of 0.4 Pa ~ 1.2 Pa, argon flow rate of 70 sccm ~ 100 sccm, substrate temperature of room temperature to 200 ° C and DC power of 100 W ~ 200 W, DC magnetron sputtering is performed on the surface of the reverse conductive layer to obtain a reverse protective layer, that is, an antistatic intelligent thermal control coating.