Nonmetal intelligent thermal control device and preparation method thereof

Abstract

The invention discloses a nonmetal intelligent thermal control device and a preparation method thereof, and belongs to the technical field of passive radiation thermal management. The invention aims to solve the problems that the processing technology of the intelligent thermal control device is limited, the service performance of the metal layer is degraded and the metal layer is adaptive to other layers due to high-temperature softening of the metal layer in the existing intelligent thermal control device. The film system structure of the non-metal intelligent thermal control device sequentially comprises an infrared reflecting layer, a first transparent dielectric layer, a phase change material layer, a second transparent dielectric layer, a third transparent dielectric layer, a functional layer and a fourth transparent dielectric layer from bottom to top, the infrared reflecting layer is ITO (Indium Tin Oxide); the first transparent dielectric layer is BaF2; the phase change material layer is a W-doped VO2 thin film; the second transparent dielectric layer is BaF2; the third transparent dielectric layer is ZnS; the functional layer is B4C; and the fourth transparent dielectric layer is ZnS. The method has a wide engineering application prospect, and particularly shows huge potential in the fields of building outer walls, heat dissipation of electronic equipment, wearable equipment and the like.

Description

Technical Field

[0001] The present invention belongs to the technical field of passive radiative thermal management, and particularly relates to a non-metallic intelligent thermal control device and a preparation method thereof. Background Art

[0002] With the increasing intensification of global climate change and energy crisis, dynamic radiative thermal management technology, as an emerging thermal control means, has gradually become one of the key technologies for solving thermal management problems in buildings, electronic devices and other fields. This technology realizes precise control of the surface temperature of an object by utilizing the ability of materials to adjust their thermal radiation characteristics under different environmental conditions. The dynamic radiative thermal management technology can automatically adjust the thermal radiation performance of materials according to the change of the external temperature, not only effectively avoiding overheating problems, but also significantly improving the energy utilization efficiency. Especially in the fields of building temperature control, electronic device heat dissipation, wearable devices, etc., this technology has shown great application potential.

[0003] Radiative thermal management devices usually rely on the combination of a metal reflective layer, a phase change functional layer and an infrared-transmitting layer. For example, Gu et al. proposed an intelligent thermal control device based on a Fabry - Perot cavity structure (VO 2 / HfO 2 / Al), with an emissivity change reaching 0.51. (J. Gu, H. Wei, F. Ren, H. Guan, S. Liang, C. Geng, L. Li, J. Zhao, S. Dou, Y. Li, ACS Appl. Mater. Interfaces, 2022, 14, 2683 - 2690). Taylor et al. fabricated a VO 2 / Si / Al intelligent emitter based on a Fabry - Perot cavity, and its emissivity (2.5 - 25 μm) increased from 0.14 at room temperature to 0.60 at 100 °C. (S. Taylor, L. Long, R. McBurney, P. Sabbaghi, J. Chao, L. Wang, Sol. Energy Mater. Sol. Cells, 2020, 217, 110739).

[0004] However, in the film stack structure of intelligent thermal control devices, the metal layer usually achieves the design goal of low temperature and low emissivity through its high reflectivity, but this structure also has some significant disadvantages. The metal layer not only limits the flexibility of the processing technology, but also may lead to poor stability of the film stack. Especially under high temperature conditions, it may pose challenges to the high temperature resistance of the overall structure. For example, the Al film cannot be stable for a long time at a high temperature of up to 500 °C. Therefore, when there is an Al film, VO 2The deposition and annealing temperatures of the functional layer shall not exceed 500 °C. The metal reflective layer also limits the performance of the material in regulating thermal radiation under different environmental conditions. In particular, melting and softening occurring under extreme temperature fluctuations may lead to a decrease in thermal control efficiency.

[0005] In addition, the metal layer usually has a large coefficient of thermal expansion and is not matched with other non-metal layers in the film system, which will affect the long-term stability of the device during thermal cycling. Therefore, developing high-performance all-non-metal intelligent thermal control devices to break through the limitations brought by the metal layer has become the key to improving the application effect of dynamic radiative thermal management technology. Summary of the Invention

[0006] The object of the present invention is to solve the problems of limited processing technology of intelligent thermal control devices caused by high-temperature softening of the metal layer in existing intelligent thermal control devices, degradation of the service performance of the metal layer, and its compatibility with other layers, and to provide a non-metal intelligent thermal control device and its preparation method.

[0007] The present invention proposes a non-metal intelligent thermal control device, aiming to optimize the processing technology of the intelligent thermal control device to break through the performance bottleneck and solve the compatibility problem between the metal layer and other functional layers to improve the service stability.

[0008] The film system structure of a non-metal intelligent thermal control device from bottom to top is successively: an infrared reflective layer, a first transparent dielectric layer, a phase change material layer, a second transparent dielectric layer, a third transparent dielectric layer, a functional layer, and a fourth transparent dielectric layer;

[0009] The infrared reflective layer is ITO;

[0010] The first transparent dielectric layer is BaF 2 ;

[0011] The phase change material layer is a W-doped VO 2 thin film;

[0012] The second transparent dielectric layer is BaF 2 ;

[0013] The third transparent dielectric layer is ZnS;

[0014] The functional layer is B 4 C;

[0015] The fourth transparent dielectric layer is ZnS.

[0016] A preparation method of a non-metal intelligent thermal control device is specifically completed according to the following steps:

[0017] I. Cleaning the substrate:

[0018] The substrate is successively placed in deionized water, absolute ethanol, and acetone and ultrasonically cleaned for a period of time respectively, and then dried with nitrogen to obtain a clean substrate;

[0019] II. Preparation of an infrared reflection layer:

[0020] Under the conditions of a background vacuum degree of 10 -3 Pa to 10 -5 Pa, a temperature of 200 °C to 300 °C, an argon gas flow rate of 70 sccm to 100 sccm, an oxygen gas flow rate of 7 sccm to 10 sccm, a gas pressure of 0.4 Pa to 0.9 Pa, and a sputtering power of 150 W to 180 W, using indium tin oxide alloy as the target, depositing an ITO thin film on the substrate by DC sputtering technology, and then annealing for a period of time in a nitrogen atmosphere at a temperature of 400 °C to 500 °C to obtain a substrate with an infrared reflection layer;

[0021] III. Preparation of the first transparent dielectric layer:

[0022] Under the conditions of a background vacuum degree of 10 -6 Pa to 10 -8 Pa, a substrate temperature of room temperature to 100 °C, a target power of 2 kW to 5 kW, and a deposition rate of Using BaF 2 powder as the evaporation material, depositing a BaF 2 thin film on the infrared reflection layer by electron beam evaporation technology to obtain a substrate with the first transparent dielectric layer;

[0023] IV. Preparation of the phase change material layer:

[0024] Under the conditions of a frequency of 400 Hz to 450 Hz, a pulse width of 50 μs to 100 μs, a power of 180 W to 200 W, a background vacuum degree of 5×10 -4 Pa to 1×10 -5 Pa, a deposition pressure of 0.4 Pa to 0.9 Pa, an argon gas flow rate of 80 sccm to 100 sccm, an oxygen gas flow rate of 1.0 sccm to 1.5 sccm, and a substrate temperature of 200 °C to 400 °C, using a tungsten-vanadium alloy as the target, depositing a W-doped VO 2 thin film on the first transparent dielectric layer by high-energy pulsed magnetron sputtering technology, and then annealing for a period of time in an argon atmosphere at a temperature of 480 °C to 580 °C to obtain a substrate with the phase change material layer;

[0025] V. Preparation of the second transparent dielectric layer:

[0026] Under the conditions of a background vacuum degree of 10 -6 Pa to 10 -8Under the conditions of Pa, substrate temperature ranging from room temperature to 100 °C, target power ranging from 2 kW to 5 kW, and deposition rate of With BaF 2 powder as the evaporation material, BaF 2 film is deposited on the phase change material layer by electron beam evaporation technology to obtain a substrate with a second transparent dielectric layer;

[0027] VI. Preparation of the third transparent dielectric layer:

[0028] Under the conditions of background vacuum degree of 10 -6 Pa to 10 -8 Pa, substrate temperature ranging from room temperature to 150 °C, target power ranging from 2 kW to 4 kW, and deposition rate of With ZnS powder as the evaporation material, ZnS film is deposited on the second transparent dielectric layer by electron beam evaporation technology to obtain a substrate with a third transparent dielectric layer;

[0029] VII. Preparation of the functional layer:

[0030] Under the conditions of background vacuum degree of 10 -6 Pa to 10 -8 Pa, substrate temperature ranging from room temperature to 150 °C, target power ranging from 2 kW to 4 kW, and deposition rate of With B 4 C powder as the evaporation material, B 4 C film is deposited on the third transparent dielectric layer by electron beam evaporation technology to obtain a substrate with a functional layer;

[0031] VIII. Preparation of the fourth transparent dielectric layer:

[0032] Under the conditions of background vacuum degree of 10 -6 Pa to 10 -8 Pa, substrate temperature ranging from room temperature to 150 °C, target power ranging from 2 kW to 4 kW, and deposition rate of With ZnS powder as the evaporation material, ZnS film is deposited on the functional layer by electron beam evaporation technology to obtain a non-metallic intelligent thermal control device.

[0033] Principle of the present invention:

[0034] In the non-metallic intelligent thermal control device described in the present invention, the functions of each layer are as follows:

[0035] ITO layer: The application of the ITO layer not only avoids the use of a metal layer, but also enhances the compatibility of the film system and reduces the thermal stress between the film layers during the thermal cycle due to its similar coefficient of thermal expansion to other non-metallic materials.

[0036] BaF 2Layer and ZnS layer: BaF 2 The layer and ZnS layer, as a transparent dielectric material with high permeability, can effectively transmit infrared light in radiative heat management.

[0037] VO 2 Layer: As a phase change material, VO 2 has significant temperature response characteristics. It can undergo a metal-insulator phase transition when the temperature changes, thereby changing its radiative emissivity. The addition of VO 2 enables the film system to have the ability to dynamically adjust thermal radiation. It can automatically adjust the thermal radiation ability according to the change of ambient temperature to achieve precise thermal control.

[0038] B 4 C layer: B 4 The C layer, as a functional layer, provides additional optical properties. It cooperates with the upper dielectric layer to regulate the spectral broadening of the full width at half maximum and also enhances the structural stability and heat resistance of the film system.

[0039] Advantages of the present invention:

[0040] First, by designing this non-metallic intelligent thermal control device, the present invention successfully weakens the limitation of the presence of the metal reflective layer on the device processing technology, avoiding problems such as its performance degradation and poor compatibility with other layers. Through precise process design and post-annealing treatment, the lower layer material has excellent stability, broadening the process window of the upper layer, enabling the preparation of a phase change layer and a functional layer with higher crystallinity at higher deposition temperatures and annealing temperatures. This improvement significantly enhances the device's thermal management ability and service stability. The change value of the infrared emissivity (2.5 - 25 μm) reaches 0.54. After the high-temperature stability test, the change value of the emissivity is 0.55. After the low-temperature stability test, the change value of the emissivity is 0.53. After the high and low temperature stability tests, the performance basically has no attenuation.

[0041] Second, the non-metallic intelligent thermal control device in the present invention avoids the use of traditional metal layers and adopts a combination of non-metallic infrared mirrors, transparent dielectric layers, and phase change materials to achieve efficient and stable dynamic radiative heat management.

[0042] Third, the present invention has broad engineering application prospects, especially showing great potential in fields such as building exteriors, heat dissipation of electronic devices, and wearable devices. Description of the Drawings

[0043] Figure 1 is a schematic structural diagram of the non-metallic intelligent thermal control device described in the present invention;

[0044] Figure 2 is the variable-temperature infrared reflection spectrum of the non-metallic intelligent thermal control device prepared in Example 1 before the high and low temperature stability test;

[0045] Figure 3 The variable-temperature infrared reflection spectrum of the non-metallic intelligent thermal control device prepared in Example 1 after the high-temperature stability test;

[0046] Figure 4 The variable-temperature infrared reflection spectrum of the non-metallic intelligent thermal control device prepared in Example 1 after the low-temperature stability test. Detailed implementation manners

[0047] Detailed implementation manner 1: The film system structure of a non-metallic intelligent thermal control device is, from bottom to top in sequence: an infrared reflection layer, a first transparent dielectric layer, a phase change material layer, a second transparent dielectric layer, a third transparent dielectric layer, a functional layer, and a fourth transparent dielectric layer;

[0048] The infrared reflection layer is ITO;

[0049] The first transparent dielectric layer is BaF 2 ;

[0050] The phase change material layer is a W-doped VO 2 thin film;

[0051] The second transparent dielectric layer is BaF 2 ;

[0052] The third transparent dielectric layer is ZnS;

[0053] The functional layer is B 4 C;

[0054] The fourth transparent dielectric layer is ZnS.

[0055] The present invention selects appropriate materials (ITO, BaF 2 , VO 2 , ZnS, B 4 C), and arranges the deposition sequence of each layer reasonably, thereby improving the thermal stability and optical performance of the film structure; by combining the electron beam evaporation technology and the magnetron sputtering technology, the high-quality deposition of the ITO thin film, BaF 2 film, VO 2 film, ZnS thin film and B 4 C thin film is successfully realized; by precisely controlling the preparation processes of each layer of thin film, the uniformity and quality of each film layer are ensured, and the problem of performance decline in practical applications is avoided.

[0056] The present invention solves the problems of metal layer processing limitations, performance degradation, and poor interlayer compatibility through a non-metal film system structure for removing the metal layer; the excellent stability of the lower layer expands the process window of the upper layer, allowing for the preparation of a higher-quality phase change layer at a higher temperature, thus breaking through the performance bottleneck of the traditional metal layer structure and improving the thermal management ability and service stability.

[0057] Specific Embodiment 2: The difference between this embodiment and Specific Embodiment 1 is that the thickness of the infrared reflection layer is 1200 nm to 1300 nm. Other steps are the same as those in Specific Embodiment 1.

[0058] Specific Embodiment 3: The difference between this embodiment and either Specific Embodiment 1 or 2 is that the thickness of the first transparent dielectric layer is 800 nm to 900 nm. Other steps are the same as those in Specific Embodiment 1 or 2.

[0059] Specific Embodiment 4: The difference between this embodiment and any one of Specific Embodiments 1 to 3 is that the thickness of the phase change material layer is 40 nm to 50 nm. Other steps are the same as those in Specific Embodiments 1 to 3.

[0060] Specific Embodiment 5: The difference between this embodiment and any one of Specific Embodiments 1 to 4 is that the thickness of the second transparent dielectric layer is 300 nm to 400 nm. Other steps are the same as those in Specific Embodiments 1 to 4.

[0061] Specific Embodiment 6: The difference between this embodiment and any one of Specific Embodiments 1 to 5 is that the thickness of the third transparent dielectric layer is 50 nm to 60 nm. Other steps are the same as those in Specific Embodiments 1 to 5.

[0062] Specific Embodiment 7: The difference between this embodiment and any one of Specific Embodiments 1 to 6 is that the thickness of the functional layer is 300 nm to 400 nm. Other steps are the same as those in Specific Embodiments 1 to 6.

[0063] Specific Embodiment 8: The difference between this embodiment and any one of Specific Embodiments 1 to 7 is that the thickness of the fourth transparent dielectric layer is 110 nm to 120 nm. Other steps are the same as those in Specific Embodiments 1 to 7.

[0064] Specific Embodiment 9: This embodiment is a preparation method of a non-metal intelligent thermal control device, which is specifically completed according to the following steps:

[0065] 1. Cleaning the substrate:

[0066] Place the substrate in deionized water, absolute ethanol, and acetone in sequence, ultrasonically clean for a period of time respectively, and then dry it with nitrogen to obtain a clean substrate;

[0067] II. Preparation of infrared reflective layer:

[0068] Under the conditions of a background vacuum of 10 -3 Pa to 10 -5 Pa, a temperature of 200°C to 300°C, an argon gas flow rate of 70 sccm to 100 sccm, an oxygen gas flow rate of 7 sccm to 10 sccm, a gas pressure of 0.4 Pa to 0.9 Pa, and a sputtering power of 150 W to 180 W, using indium tin oxide alloy as the target, depositing an ITO thin film on the substrate by DC sputtering technology, and then annealing for a period of time in a nitrogen atmosphere at a temperature of 400°C to 500°C to obtain a substrate with an infrared reflective layer;

[0069] III. Preparation of the first transparent dielectric layer:

[0070] Under the conditions of a background vacuum of 10 -6 Pa to 10 -8 Pa, a substrate temperature of room temperature to 100°C, a target power of 2 kW to 5 kW, and a deposition rate of Using BaF 2 powder as the evaporation material, depositing a BaF 2 thin film on the infrared reflective layer by electron beam evaporation technology to obtain a substrate with the first transparent dielectric layer;

[0071] IV. Preparation of the phase change material layer:

[0072] Under the conditions of a frequency of 400 Hz to 450 Hz, a pulse width of 50 μs to 100 μs, a power of 180 W to 200 W, a background vacuum of 5×10 -4 Pa to 1×10 -5 Pa, a deposition pressure of 0.4 Pa to 0.9 Pa, an argon gas flow rate of 80 sccm to 100 sccm, an oxygen gas flow rate of 1.0 sccm to 1.5 sccm, and a substrate temperature of 200°C to 400°C, using tungsten-vanadium alloy as the target, depositing a W-doped VO 2 thin film on the first transparent dielectric layer by high-energy pulsed magnetron sputtering technology, and then annealing for a period of time in an argon atmosphere at a temperature of 480°C to 580°C to obtain a substrate with the phase change material layer;

[0073] V. Preparation of the second transparent dielectric layer:

[0074] Under the conditions of a background vacuum of 10 -6 Pa to 10 -8 Pa, a substrate temperature of room temperature to 100°C, a target power of 2 kW to 5 kW, and a deposition rate of Using BaF 2 powder as the evaporation material, depositing a BaF2 A thin film is obtained, and a substrate containing a second transparent dielectric layer is obtained;

[0075] VI. Preparation of a third transparent dielectric layer:

[0076] Under the conditions of a background vacuum degree of 10 -6 Pa to 10 -8 Pa, a substrate temperature of room temperature to 150 °C, a target power of 2 kW to 4 kW, and a deposition rate of Using ZnS powder as the evaporation material, a ZnS thin film is deposited on the second transparent dielectric layer by electron beam evaporation technology, and a substrate containing a third transparent dielectric layer is obtained;

[0077] VII. Preparation of a functional layer:

[0078] Under the conditions of a background vacuum degree of 10 -6 Pa to 10 -8 Pa, a substrate temperature of room temperature to 150 °C, a target power of 2 kW to 4 kW, and a deposition rate of Using B 4 C powder as the evaporation material, a B 4 C thin film is deposited on the third transparent dielectric layer by electron beam evaporation technology, and a substrate containing a functional layer is obtained;

[0079] VIII. Preparation of a fourth transparent dielectric layer:

[0080] Under the conditions of a background vacuum degree of 10 -6 Pa to 10 -8 Pa, a substrate temperature of room temperature to 150 °C, a target power of 2 kW to 4 kW, and a deposition rate of Using ZnS powder as the evaporation material, a ZnS thin film is deposited on the functional layer by electron beam evaporation technology, and a non-metallic intelligent thermal control device is obtained.

[0081] Specific Embodiment X: The difference between this embodiment and one of Embodiments 1 to 9 is that: the substrate described in Step 1 is quartz; in Step 1, the substrate is successively placed in deionized water, absolute ethanol, and acetone and ultrasonically cleaned for 20 min to 30 min respectively; the annealing time described in Step 2 is 1 h to 3 h; the annealing time described in Step 4 is 2 h to 6 h; the atomic fraction of tungsten in the tungsten-vanadium alloy described in Step 4 is 2%. Other steps are the same as those in Embodiments 1 to 9.

[0082] The following examples are used to verify the beneficial effects of the present invention:

[0083] Example 1: The film structure of a non-metal intelligent thermal control device from bottom to top is successively: an infrared reflection layer, a first transparent dielectric layer, a phase change material layer, a second transparent dielectric layer, a third transparent dielectric layer, a functional layer, and a fourth transparent dielectric layer;

[0084] The infrared reflection layer is ITO with a thickness of 1285 nm;

[0085] The first transparent dielectric layer is BaF 2 with a thickness of 872 nm;

[0086] The phase change material layer is a W-doped VO 2 thin film with a thickness of 47 nm;

[0087] The second transparent dielectric layer is BaF 2 with a thickness of 364 nm;

[0088] The third transparent dielectric layer is ZnS with a thickness of 51 nm;

[0089] The functional layer is B 4 C with a thickness of 389 nm;

[0090] The fourth transparent dielectric layer is ZnS with a thickness of 113 nm;

[0091] The preparation method of the non-metal intelligent thermal control device is specifically completed according to the following steps:

[0092] I. Cleaning the substrate:

[0093] Place the substrate in deionized water, absolute ethanol, and acetone in sequence and ultrasonically clean for 20 min each, then blow dry with nitrogen to obtain a clean substrate;

[0094] The substrate described in step I is quartz;

[0095] II. Preparing the infrared reflection layer:

[0096] Under the conditions of a background vacuum degree of 1×10 -5 Pa, a temperature of 300 °C, an argon gas flow rate of 80 sccm, an oxygen gas flow rate of 8 sccm, a gas pressure of 0.9 Pa, and a sputtering power of 150 W, using indium tin oxide alloy as the target, deposit an ITO thin film on the substrate by DC sputtering technology, and then anneal for a period of time in a nitrogen atmosphere at a temperature of 400 °C to obtain a substrate with an infrared reflection layer;

[0097] The annealing time described in step II is 2 h;

[0098] III. Preparing the first transparent dielectric layer:

[0099] Under the conditions of a background vacuum of 1×10 -6 Pa, a substrate temperature of room temperature, a target power of 2 kW, and a deposition rate of BaF 2 powder as the evaporation material, BaF 2 thin film was deposited on the infrared reflective layer by electron beam evaporation technology to obtain a substrate containing the first transparent dielectric layer;

[0100] IV. Preparation of the phase change material layer:

[0101] Under the conditions of a frequency of 400 Hz, a pulse width of 70 μs, a power of 180 W, a background vacuum of 5×10 -4 Pa, a deposition pressure of 0.4 Pa, an argon flow rate of 80 sccm, an oxygen flow rate of 1.5 sccm, and a substrate temperature of 200 °C, a tungsten-vanadium alloy was used as the target, and W-doped VO 2 thin film was deposited on the first transparent dielectric layer by high-energy pulsed magnetron sputtering technology, and then annealed in an argon atmosphere at a temperature of 500 °C for a period of time to obtain a substrate containing the phase change material layer;

[0102] The annealing time described in step IV is 6 h;

[0103] The atomic fraction of tungsten in the tungsten-vanadium alloy described in step IV is 2%;

[0104] V. Preparation of the second transparent dielectric layer:

[0105] Under the conditions of a background vacuum of 1×10 -6 Pa, a substrate temperature of room temperature, a target power of 2 kW, and a deposition rate of BaF 2 powder as the evaporation material, BaF 2 thin film was deposited on the phase change material layer by electron beam evaporation technology to obtain a substrate containing the second transparent dielectric layer;

[0106] VI. Preparation of the third transparent dielectric layer:

[0107] Under the conditions of a background vacuum of 1×10 -6 Pa, a substrate temperature of room temperature, a target power of 2 kW, and a deposition rate of ZnS powder as the evaporation material, ZnS thin film was deposited on the second transparent dielectric layer by electron beam evaporation technology to obtain a substrate containing the third transparent dielectric layer;

[0108] VII. Preparation of the functional layer:

[0109] Under the conditions of a background vacuum of 1×10 -6 Pa, a substrate temperature of 150 °C, a target power of 4 kW, and a deposition rate of Under the condition of, with B 4 C powder as the evaporation material, deposit BC 4 film on the third transparent dielectric layer by electron beam evaporation technology to obtain a substrate with a functional layer;

[0110] VIII. Preparation of the fourth transparent dielectric layer:

[0111] Under the condition of a background vacuum of 1×10 -6 Pa, a substrate temperature of room temperature, a target power of 2 kW, and a deposition rate of , deposit ZnS film on the functional layer with ZnS powder as the evaporation material by electron beam evaporation technology to obtain a non-metallic intelligent thermal control device.

[0112] Use a self-made temperature control device with heating and cooling modes to adjust the temperature of the sample. According to repeated measurements, the temperature error of the sample is less than 0.5 °C. The temperature is measured by a thermocouple in contact with the regulator. During the test, the temperature of the device is controlled at 0 °C and 60 °C respectively, and the infrared reflection spectrum is measured by a Vertex 70 Fourier transform infrared spectrometer using an A562 integrating sphere.

[0113] According to Kirchhoff's law, the infrared emissivity can be calculated from the reflection spectrum using the following two equations:

[0114]

[0115] where c 1 represents the first radiation constant, c 2 represents the second radiation constant, λ represents the wavelength, and T represents the temperature. The change value of the emissivity is the difference between the high-temperature and low-temperature emissivities.

[0116] Figure 2 is the variable-temperature infrared reflection spectrum of the device before the high and low temperature stability test of the non-metallic intelligent thermal control device prepared in Example 1;

[0117] From Figure 2 it can be seen that the change value of the emissivity of the non-metallic intelligent thermal control device prepared in Example 1 is 0.54.

[0118] Perform a 1-hour high-temperature treatment on the device in a tube furnace at 500 °C in an argon atmosphere, re-measure the spectrum of the device and calculate the emissivity. The conditions for spectral testing and emissivity calculation are the same as above.

[0119] Figure 3 is the variable-temperature infrared reflection spectrum of the device after the high-temperature stability test of the non-metallic intelligent thermal control device prepared in Example 1;

[0120] From Figure 3It can be known that the change value of the emissivity after the high-temperature stability test of the non-metallic intelligent thermal control device prepared in Example 1 is 0.55.

[0121] Immerse the device in liquid nitrogen and perform low-temperature treatment for 1 hour. Re-measure the spectrum of the device and calculate the emissivity. The conditions for spectral testing and emissivity calculation are the same as above.

[0122] Figure 4 It is the variable-temperature infrared reflection spectrum of the device after the low-temperature stability test of the non-metallic intelligent thermal control device prepared in Example 1;

[0123] From Figure 4 It can be known that after the low-temperature stability test of the non-metallic intelligent thermal control device prepared in Example 1, the change value of the emissivity is 0.53.

[0124] Example 2: The difference between this example and Example 1 is that the infrared reflection layer is ITO with a thickness of 1371 nm;

[0125] The first transparent dielectric layer is BaF 2 , with a thickness of 929 nm;

[0126] The phase change material layer is a W-doped VO 2 thin film with a thickness of 50 nm;

[0127] The second transparent dielectric layer is BaF 2 , with a thickness of 342 nm;

[0128] The third transparent dielectric layer is ZnS with a thickness of 49 nm;

[0129] The functional layer is B 4 C with a thickness of 405 nm;

[0130] The fourth transparent dielectric layer is ZnS with a thickness of 287 nm. Other steps and parameters are the same as those in Example 1.

[0131] The change value of the infrared emissivity (2.5 - 25 μm) of the non-metallic intelligent thermal control device prepared in Example 2 reaches 0.49, the change value of the emissivity after the high-temperature stability test is 0.49, and after the low-temperature stability test, the change value of the emissivity is 0.48.

Claims

1. A non-metallic intelligent thermal control device, characterized in that A film structure of a non-metallic intelligent thermal control device is, from bottom to top, an infrared reflection layer, a first transparent medium layer, a phase change material layer, a second transparent medium layer, a third transparent medium layer, a functional layer, and a fourth transparent medium layer; The infrared reflection layer is ITO; The first transparent medium layer is BaF2; The phase change material layer is a W-doped VO2 thin film; The second transparent medium layer is BaF2; The third transparent medium layer is ZnS; The functional layer is B4C; The fourth transparent medium layer is ZnS.

2. A non-metallic intelligent thermal control device according to claim 1, characterized in that The thickness of the infrared reflection layer is 1200nm-1300nm.

3. A non-metallic intelligent thermal control device according to claim 1, characterized in that The thickness of the first transparent medium layer is 800nm-900nm.

4. A non-metallic intelligent thermal control device according to claim 1, characterized in that The thickness of the phase change material layer is 40nm-50nm.

5. The non-metallic intelligent thermal control device according to claim 1, characterized in that The thickness of the second transparent medium layer is 300nm-400nm.

6. The non-metallic intelligent thermal control device according to claim 1, characterized in that The thickness of the third transparent medium layer is 50nm-60nm.

7. The non-metallic intelligent thermal control device according to claim 1, characterized in that The thickness of the functional layer is 300nm-400nm.

8. The non-metallic intelligent thermal control device according to claim 1, characterized in that The thickness of the fourth transparent medium layer is 110nm-120nm.

9. The method for preparing a non-metallic intelligent thermal control device according to claim 1, characterized in that The preparation method is specifically completed according to the following steps:

1. Cleaning the substrate: The substrate is placed in deionized water, anhydrous ethanol and acetone for ultrasonic cleaning for a period of time, and then blown dry with nitrogen to obtain a clean substrate; 2. Preparation of infrared reflection layer: At a background vacuum of 10 -3 Pa~10 -5 Under the conditions of 0.4 Pa to 0.9 Pa, temperature of 200° C. to 300° C., argon gas flow rate of 70 sccm to 100 sccm, oxygen gas flow rate of 7 sccm to 10 sccm, gas pressure of 0.4 Pa to 0.9 Pa and sputtering power of 150 W to 180 W, a conductive indium tin alloy is used as a target material, and an ITO film is deposited on a substrate by a DC sputtering technique, and then annealed for a period of time in a nitrogen atmosphere at a temperature of 400° C. to 500° C. to obtain a substrate containing an infrared reflection layer; 3. Preparation of the first transparent medium layer: At a background vacuum of 10 -6 Pa~10 -8 Pa, substrate temperature is room temperature ~ 100 ° C, target power is 2kW ~ 5kW, deposition rate is Under the condition of , using BaF2 powder as evaporation material, electron beam evaporation technology is used to deposit BaF2 thin film on the infrared reflection layer to obtain a substrate containing a first transparent medium layer; 4. Preparation of phase change material layer: At a frequency of 400 Hz to 450 Hz, a pulse width of 50 μs to 100 μs, a power of 180 W to 200 W, and a background vacuum of 5 × 10 -4 Pa~1×10 -5 Under the conditions of 0.4Pa-0.9Pa, deposition pressure of 0.4Pa-0.9Pa, argon flow rate of 80sccm-100sccm, oxygen flow rate of 1.0sccm-1.5sccm and substrate temperature of 200℃-400℃, a tungsten-vanadium alloy is used as a target, and a W-doped VO2 thin film is deposited on the first transparent dielectric layer by high-energy pulsed magnetron sputtering technology, and then annealed for a period of time in an argon atmosphere at a temperature of 480℃-580℃ to obtain a substrate containing a phase change material layer; 5. Preparation of the second transparent medium layer: At a background vacuum of 10 -6 Pa~10 -8 Pa, substrate temperature is room temperature ~ 100 ° C, target power is 2kW ~ 5kW, deposition rate is Under the condition of , using BaF2 powder as evaporation material, electron beam evaporation technology is used to deposit BaF2 thin film on the phase change material layer to obtain a substrate containing a second transparent medium layer; 6. Preparation of the third transparent medium layer: At a background vacuum of 10 -6 Pa~10 -8 Pa, substrate temperature is room temperature ~ 150 ° C, target power is 2kW ~ 4kW, deposition rate is Under the condition of , using ZnS powder as evaporation material, an electron beam evaporation technique is used to deposit a ZnS thin film on the second transparent medium layer, thereby obtaining a substrate containing a third transparent medium layer; 7. Preparation of functional layer: At a background vacuum of 10 -6 Pa~10 -8 Pa, substrate temperature is room temperature ~ 150 ° C, target power is 2kW ~ 4kW, deposition rate is Under the condition of , using B4C powder as evaporation material, electron beam evaporation technology is used to deposit B4C thin film on the third transparent medium layer to obtain a substrate containing a functional layer; 8. Preparation of the fourth transparent medium layer: At a background vacuum of 10 -6 Pa~10 -8 Pa, substrate temperature is room temperature ~ 150 ° C, target power is 2kW ~ 4kW, deposition rate is Under the conditions of , ZnS powder was used as the evaporation material, and electron beam evaporation technology was used to deposit ZnS film on the functional layer to obtain a non-metallic intelligent thermal control device.

10. The method for preparing a non-metallic intelligent thermal control device according to claim 9, characterized in that The substrate described in step one is quartz; in step one, the substrate is placed in deionized water, anhydrous ethanol and acetone in turn and ultrasonically cleaned for 20 minutes to 30 minutes respectively; the annealing time described in step two is 1 hour to 3 hours; the annealing time described in step four is 2 hours to 6 hours; the atomic fraction of tungsten in the tungsten-vanadium alloy described in step four is 2%.

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