An electrically-driven wide-spectrum invisibility system

Abstract

The present application relates to a kind of electric drive-based wide spectrum stealth system.The electric drive-based wide spectrum stealth system, including the base body, multilayer composite electrode, electrochromic layer, gel electrolyte layer and transparent electrode that are sequentially stacked;The multilayer composite electrode is composed of first transparent semiconductor layer / precious metal layer / second transparent semiconductor layer.

Description

Technical Field

[0001] This invention relates to an electrically driven broadband stealth system, belonging to the field of chemical material synthesis and functional materials technology. Background Technology

[0002] Variable emissivity materials are materials whose emissivity can be controlled by external fields (such as electric fields, temperature fields, etc.), thus possessing a certain ability to adapt to changes in environmental background and achieving infrared dynamic stealth for targets. Currently, the most researched variable emissivity materials are mainly divided into thermochromic and electrochromic types. Thermochromic materials mainly include perovskite-doped manganeseates and vanadium dioxide, while electrochromic materials mainly include tungsten trioxide (WO3), polyaniline (PANI), and polythiophene and its derivatives. The application of electrochromic emissivity materials is in the form of electrochromic emissivity devices. Figure 1 This is a schematic diagram of an electrovariable emissivity device. When an electrical signal is applied to the low-emissivity electrode layer, the emissivity of the variable emissivity material layer is adjusted accordingly. Compared to thermochromic devices, the applied electrical signal is simple, continuous, and controllable, allowing for continuous adjustment of the emissivity of the variable emissivity material. Furthermore, the emissivity adjustment range of electrovariable emissivity materials can reach 0.1–0.8, far exceeding that of thermochromic devices. Therefore, electrovariable emissivity devices have become a research hotspot in infrared dynamic stealth technology, with the expectation of its application in next-generation stealth aircraft. In addition, electrovariable emissivity devices also have very broad application prospects in spacecraft thermal control.

[0003] According to Kirchhoff's laws and the laws of absorption, reflection, and transmission, the emissivity of a general material is equal to its corresponding absorptivity, and the sum of absorptivity, reflectivity, and transmittance is one. A material with high emissivity will exhibit low reflectivity and transmittance, and vice versa. For variable emissivity materials used in infrared stealth technology, a higher reflectivity when emissivity is reduced can significantly reduce the infrared radiation of the target. Combined with a high emissivity state, this allows for greater adjustment of the target's infrared radiation characteristics.

[0004] Furthermore, electrically driven color changes can aid in achieving visual stealth for equipment. Clearly, the more colors that can be changed, the more diverse the operating environments and the wider the application areas of the equipment. However, current electrically driven systems often only allow switching between two colors, and it is difficult to achieve coordinated changes in near-infrared emissivity and color. Summary of the Invention

[0005] To address the limitations of existing stealth systems, such as narrow adjustment range and slow response speed, this invention provides an electrically driven broadband stealth system, comprising a substrate, a multilayer composite electrode, an electrochromic layer, a gel electrolyte layer, and a transparent electrode stacked sequentially; the multilayer composite electrode is composed of a first transparent semiconductor layer / noble metal layer / second transparent semiconductor layer.

[0006] Compared to other devices that control color or near-infrared emissivity, the electrically driven broadband stealth system designed in this patent can simultaneously adjust color and the near-infrared region. It boasts not only a fast response speed but also a simple fabrication process, facilitating assembly and offering broad application prospects. Specifically, based on the mutual interference between a first transparent semiconductor / noble metal / second transparent semiconductor, controllable and reversible switching of multiple colors can be achieved. The three-layer composite electrode not only has better conductivity, improving the device's response speed, but also, through Fabry-Perot interference, enables the reflected light to have a narrower frequency band, thus exhibiting color. When the device changes color under an external voltage driving force, the refractive index n and extinction coefficient k of the electrochromic layer material change, thereby synergistically interacting with the composite electrode. Depending on the values ​​of n and k, the device can reflect different light, exhibiting different colors.

[0007] Preferably, the substrate is a silicon wafer substrate, a transparent glass substrate, or a metal substrate.

[0008] Preferably, the materials of the first transparent semiconductor layer and the second transparent semiconductor layer are independently selected from one of ITO, FTO and AZO; the material of the noble metal layer is selected from at least one of Ag, Au, Pt and Pd.

[0009] Preferably, the thickness of the first transparent semiconductor layer is 50-500 nm, the thickness of the noble metal layer is 1-10 nm, and the thickness of the second transparent semiconductor layer is 10-100 nm.

[0010] Preferably, the electrochromic layer is made of WO3 material. 3-x (0<x≤0.3, preferably 0.02≤x≤0.3), at least one of V2O5, MoO3, Bruce Blue and TiO2; the thickness of the electrochromic layer is 100~500nm.

[0011] Preferably, the transparent electrode is selected from at least one of transparent conductive oxide and metal nanowires; the surface sheet resistance of the transparent electrode is 10–40 Ω / cm. 2 Transmittance ≥75%.

[0012] Preferably, the gel electrolyte layer comprises a host material and a cationic salt distributed in the host material, wherein the host material is an amino-terminated polyimide resin; preferably, the molar ratio of the cationic salt to the amino-terminated polyimide resin is (2%-5%):1.

[0013] The cation salt is selected from at least one of Al salt, Li salt and Na salt, and preferably from at least one of aluminum perchlorate, potassium perchlorate and sodium perchlorate;

[0014] The thickness of the gel electrolyte layer is 10–100 μm, preferably 10–80 μm. A near-infrared transmitting electrolyte based on polyimide is designed to achieve a wide range of modulation of near-infrared emissivity.

[0015] Preferably, the method for preparing the gel electrolyte layer includes:

[0016] (1) Dissolve the cationic salt in an organic solvent to obtain a cationic salt solution;

[0017] (2) Add the dianhydride monomer and the diamine monomer to the cationic salt solution and mix to obtain an amino-terminated polyamic acid solution;

[0018] (3) Add crosslinking agent, dehydrating agent and catalyst to amino-terminated polyamic acid solution and mix to obtain mixed solution;

[0019] (4) The mixed solution is coated onto the substrate and left to stand at 30-80°C for 10 min-2 h to obtain the gel electrolyte layer.

[0020] Preferably, the organic solvent is at least one selected from propylene carbonate, diethyl carbonate (DEC), dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), and dimethyl glycol ether (DME); the concentration of the cation salt solution is 0.5–2 mol / L.

[0021] The total mass ratio of the dianhydride monomer and the diamine monomer to the cationic salt solution is 1:(5-20);

[0022] The molar ratio between the dianhydride monomer and the diamine monomer is n:(n+1), where n≥50;

[0023] Preferably, the dianhydride monomer is selected from at least one of pyromellitic dianhydride, benzophenone tetracarboxylic dianhydride, and diphenyl ether tetracarboxylic dianhydride, and the diamine monomer is selected from at least one of hexylene diamine, decylene diamine, diaminodiphenylmethane, diaminodiphenyl ether, p-phenylenediamine, m-phenylenediamine, m-toluenediamine, and diaminodiphenyl sulfone. The molar ratio of the dianhydride monomer to the diamine monomer affects the final degree of polymerization and the chain length of the resin. A higher degree of polymerization results in a longer resin chain, which affects not only the strength of the electrolyte layer but also the ion migration performance. In this patent, ion migration performance is more important than that of the electrolyte layer; therefore, a molar ratio greater than 50 is sufficient. A ratio less than 50 makes it difficult to polymerize into a stable device.

[0024] Preferably, the crosslinking agent is selected from at least one of triglycidyl-p-aminophenol, triglycidyl-triisocyanate, tetraglycidyl-diaminodiphenylmethane, tetraglycidyl-diphenyldiamine, and pyromellitic acid chloride, and the amount added is 1% to 5% of the total mass of the amino-terminated polyamic acid solution.

[0025] The dehydrating agent is selected from at least one of acetic anhydride, propionic anhydride, valeric anhydride, and dimethyl ketone, and the amount added is 0.5% to 5% of the total mass of the amino-terminated polyamic acid solution.

[0026] The catalyst is selected from at least one of pyridine, 4-methylpyridine, 3,4-dimethylpyridine, isoquinoline, and triethylamine, and the amount added is 0.1% to 1% of the total mass of the amino-terminated polyamic acid solution.

[0027] Preferably, a driving voltage is applied to an electrically driven broadband stealth system, which achieves at least three color variations and has an average emissivity between 0.1 and 0.8 in the near-infrared range of 780 nm to 2500 nm; preferably, the driving voltage is +2V to -4V.

[0028] The beneficial effects of this invention are:

[0029] 1. The electric-driven stealth system prepared by this invention can achieve changes in the emissivity spectrum of visible light color and infrared light, thereby achieving visual stealth and radar detection stealth of equipment in a wide spectral range from visible light to near-infrared light.

[0030] 2. Electrically driven stealth systems have significant advantages in terms of fast response speed and precise control;

[0031] 3. Electrically driven stealth systems are highly adaptable, have simple processing technology, are easy to assemble, and have excellent prospects for widespread application. Attached Figure Description

[0032] Figure 1This is a schematic diagram of the structure of the electrically driven broadband stealth system of the present invention;

[0033] Figure 2 This refers to the response speed and adjustment capability of the electrically driven broadband stealth system in Example 1. Detailed Implementation

[0034] The present invention will be further illustrated by the following embodiments. It should be understood that the following embodiments are for illustrative purposes only and are not intended to limit the present invention.

[0035] In this field, design-based structures enable changes in the system's color and near-infrared emissivity, allowing the equipment to blend into the ambient background and responsively adjust its emissivity.

[0036] To address the aforementioned issues, this patent presents a broadband stealth system that utilizes a multilayer composite electrode and a gel electrolyte to fabricate an electrically driven system that synergistically alters color and near-infrared emissivity. This invention achieves controllable and reversible color variations through a composite electrode structure and allows for controllable adjustment of near-infrared emissivity by introducing an infrared-transmitting electrolyte.

[0037] Specifically, the structure of the electrically driven broadband stealth system consists of a substrate, a multilayer composite electrode, an electrochromic layer, a high-strength gel electrolyte layer, and a transparent electrode stacked sequentially.

[0038] In an optional embodiment, the gel electrolyte layer is primarily composed of amino-terminated polyimide. By controlling the degree of polymerization of the monomers, the intermolecular cohesion and coordination number are increased, synergistically enhancing the resin strength and ion migration ability. It can also adjust the color and emissivity of the electrolyte over a broad spectral band. The gel electrolyte layer is a cation-conducting layer based on an organic resin, wherein the cation is H+. + Al 3+ Li + and Na + At least one of them.

[0039] In optional embodiments, the electrochromic layer is prepared by methods such as magnetron sputtering, laser pulse deposition, molecular beam epitaxy, spin coating, spraying, or dip coating.

[0040] In this invention, the DC magnetron sputtering system used for magnetron sputtering deposition may include a deposition chamber, a sample inlet chamber, several target heads, a substrate, a DC current source, and a series of mechanical pumps and vacuum pumps. The target heads are at a certain angle to the substrate and separated by a certain distance. The DC power supply is connected to the target heads. The substrate is ultrasonically cleaned with acetone, anhydrous ethanol, and deionized water for 20 minutes each, and then dried with compressed air. A portion of the conductive substrate is covered with high-temperature tape as an electrode and fixed to the substrate tray. The substrate is placed in the sample inlet chamber, and the mechanical pump is turned on to evacuate to below 5 Pa. Then, the baffle valve is opened, and the vacuum level (baseline vacuum) reaches 10. -4 Splash chambers with Pa and below.

[0041] A suitable substrate is selected based on the application scenario and field. A multilayer composite electrode of a first transparent semiconductor / noble metal / second transparent semiconductor is continuously fabricated on the substrate surface using magnetron sputtering. ITO and Ag are used as targets, argon is used as the sputtering gas, the total pressure is 0.5–2.0 Pa, the oxygen partial pressure is 0–50%, the distance between the target and the substrate is 10–20 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 30–150 W or the power density is 0.6–3.0 W / cm². 2 A multilayer composite electrode of suitable thickness is obtained by using a DC power supply on the surface.

[0042] Using tungsten, molybdenum, vanadium, or titanium as the target material, and argon and oxygen as the sputtering gas, the total pressure is 0.5–2.0 Pa, the oxygen partial pressure is 0–50%, the distance between the target and the substrate is 10–20 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 30–150 W or the power density is 0.6–3.0 W / cm³. 2 An electrochromic layer film with a thickness of 100 nm to 500 nm is deposited using a DC power supply on the surface.

[0043] Prepare a cation salt solution with a concentration of 0.5–2 mol / L (e.g., 1 mol / L). The solvent is propylene carbonate, and the solute is at least one of lithium perchlorate, sodium perchlorate, sodium chloride, and lithium chloride.

[0044] A viscous polyamic acid solution is obtained by dissolving dianhydride monomer and diamine monomer in a cationic salt solution and stirring for 10-50 minutes. The mass ratio of added monomer to cationic salt solution is 1:(5-20), and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), where n≥50. A crosslinking agent, dehydrating agent, and catalyst are added sequentially to the above amino-terminated polyamic acid solution in a ratio of 1:(1%-5%):(0.5%-5%):(0.1%-1%), and the mixture is stirred for 2-20 minutes to obtain a mixed solution.

[0045] After coating the surface of the electrochromic layer with the mixed solution (30-80℃ for 10 min-2 h), an ITO transparent electrode was placed on top. After the device cured, excess organic matter on the device surface was removed using an organic solvent. This completes the fabrication process for a high-strength gel-based flexible electrochromic layer.

[0046] The following examples further illustrate the present invention in detail. It should also be understood that the following examples are only for further explanation of the present invention and should not be construed as limiting the scope of protection of the present invention. Any non-essential improvements and adjustments made by those skilled in the art based on the above description of the present invention are within the scope of protection of the present invention. The specific process parameters, etc., in the following examples are merely examples within a suitable range; that is, those skilled in the art can make appropriate selections within the appropriate range based on the description herein, and are not intended to be limited to the specific values ​​in the examples below.

[0047] Example 1

[0048] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas, with a total pressure of 1 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 100 W applied to the target, a sputtering time of 1 h, and a thickness of 400 nm. For the noble metal, argon was used as the sputtering gas, with a total pressure of 0.6 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 20 W applied to the target, a sputtering time of 2 min, and a thickness of 5 nm. The second transparent semiconductor uses argon as the sputtering gas, with a total pressure of 1 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 70 W applied to the target, a sputtering time of 10 min, and a thickness of 80 nm. Alternatively, tungsten is used as the target, with argon and oxygen as the sputtering gases, a total pressure of 2.0 Pa, an oxygen partial pressure of 6%, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, and a DC power of 70 W or a power density of 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0049] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0050] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0051] Example 2

[0052] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 10 min, and an inorganic electrochromic layer film with a thickness of about 100 nm was obtained.

[0053] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0054] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0055] Example 3

[0056] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 45 min, and an inorganic electrochromic layer film with a thickness of about 500 nm was obtained.

[0057] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0058] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0059] Example 4

[0060] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0061] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0062] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 10 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0063] Example 5

[0064] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0065] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0066] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using an 80 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0067] Example 6

[0068] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0069] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexanediamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=500. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0070] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0071] Example 7

[0072] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0073] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexanediamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=1000. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0074] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0075] Example 8

[0076] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets, respectively. For the first transparent semiconductor, argon was used as the sputtering gas, with a total pressure of 1 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 100 W applied to the target, a sputtering time of 1.2 h, and a thickness of 500 nm. For the noble metal, argon was used as the sputtering gas, with a total pressure of 0.6 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 20 W applied to the target, a sputtering time of 3 min, and a thickness of 10 nm. The second transparent semiconductor uses argon as the sputtering gas, with a total pressure of 1 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 70 W applied to the target, a sputtering time of 15 min, and a thickness of 100 nm. Alternatively, tungsten is used as the target, with argon and oxygen as the sputtering gases, a total pressure of 2.0 Pa, an oxygen partial pressure of 6%, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, and a DC power of 70 W or a power density of 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0077] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0078] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0079] Example 9

[0080] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas, with a total pressure of 1 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 100 W applied to the target, a sputtering time of 30 min, and a thickness of 200 nm. For the noble metal, argon was used as the sputtering gas, with a total pressure of 0.6 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 20 W applied to the target, a sputtering time of 1 min, and a thickness of 2 nm. The second transparent semiconductor uses argon as the sputtering gas, with a total pressure of 1 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 70 W applied to the target, a sputtering time of 5 min, and a thickness of 20 nm. Alternatively, tungsten is used as the target, with argon and oxygen as the sputtering gases, a total pressure of 2.0 Pa, an oxygen partial pressure of 6%, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, and a DC power of 70 W or a power density of 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0081] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0082] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0083] Example 10

[0084] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0085] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is sodium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexanediamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0086] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0087] Example 11

[0088] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0089] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is aluminum perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexanediamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0090] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0091] Example 12

[0092] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0093] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexanediamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:1%:0.5%:0.1% in sequence and stir for 10 minutes to obtain a mixed solution;

[0094] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0095] Example 13

[0096] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0097] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:5%:5%:1% in sequence and stir for 10 minutes to obtain a mixed solution;

[0098] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0099] Example 14

[0100] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0101] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=30. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0102] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0103] Example 15

[0104] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0105] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:5, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0106] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0107] Example 16

[0108] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 minutes each. Then, it was fixed to the substrate tray with high-temperature tape, placed in the sample injection chamber, and the mechanical pump was turned on to pump the sample to below 5 Pa. The baffle valve was then opened to introduce a vacuum (baseline vacuum) to reach 10. -4 In a sputtering chamber with a pressure below Pa, multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, argon was used as the sputtering gas at a total pressure of 1 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, and the sputtering time was 1 h. For the noble metal, argon was used as the sputtering gas at a total pressure of 0.6 Pa, the target-substrate distance was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, and the sputtering time was 2 min. For the second transparent semiconductor, the sputtering gas is argon, the total pressure is 1 Pa, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target is 70 W, and the sputtering time is 10 min. Alternatively, using tungsten as the target, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the target-substrate distance is 15 cm, the initial substrate temperature is room temperature, and the DC power applied to the target is 70 W or the power density is 1.54 W / cm². 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0109] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexanediamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:20, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=30. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0110] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0111] Comparative Example 1

[0112] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned for 20 min each with acetone, ethanol, and deionized water. It was then fixed to a substrate tray with high-temperature tape and placed in the sample injection chamber. The mechanical pump was turned on to evacuate the sample to below 5 Pa, and the baffle valve was opened to introduce it into a sputtering chamber with a vacuum level (baseline vacuum) below 10⁻⁴ Pa. Multilayer composite electrodes and electrochromic layers were continuously deposited on the surface using magnetron sputtering. ITO and tungsten metal were used as the targets, respectively. The first transparent semiconductor uses argon as the sputtering gas, with a total pressure of 1 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 100 W applied to the target, a sputtering time of 1 h, and a thickness of 400 nm. The second transparent semiconductor uses argon as the sputtering gas, with a total pressure of 1 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 70 W applied to the target, a sputtering time of 10 min, and a thickness of 80 nm. Alternatively, tungsten is used as the target, with argon and oxygen as the sputtering gases, a total pressure of 2.0 Pa, an oxygen partial pressure of 6%, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, and a DC power of 70 W or a power density of 1.54 W / cm² applied to the target. 2 The deposition time was 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm was obtained.

[0113] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0114] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0115] Comparative Example 2

[0116] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 min, then fixed on the substrate tray with high-temperature tape and placed in the sample injection chamber. The mechanical pump was turned on to pump the sample to below 5 Pa, and the baffle valve was opened to send it into a sputtering chamber with a vacuum level (base vacuum) below 10⁻⁴ Pa. Multilayer composite electrodes and electrochromic layers were continuously deposited on the surface of the substrate by magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, the sputtering gas was argon, the total pressure was 1 Pa, the distance between the target and the substrate was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, the sputtering time was 1 h, and the thickness was 400 nm. For the noble metal, the sputtering gas was argon, the total pressure was 0.6 Pa, the distance between the target and the substrate was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, the sputtering time was 2 min, and the thickness was 5 nm. Using tungsten metal as the target material, the sputtering gas is argon and oxygen, the total pressure is 2.0 Pa, the oxygen partial pressure is 6%, the distance between the target material and the substrate is 15 cm, the initial substrate temperature is room temperature, the DC power applied to the target material is 70 W or the power density is 1.54 W / cm2, the deposition time is 30 min, and an inorganic electrochromic layer film with a thickness of about 350 nm is obtained.

[0117] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0118] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and left to stand (50 °C and 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. The resulting electrically driven broadband stealth system was thus obtained.

[0119] Comparative Example 3

[0120] (1) First, using a Si wafer as the substrate, the substrate was ultrasonically cleaned with acetone, ethanol, and deionized water for 20 min, then fixed on the substrate tray with high-temperature tape and placed in the sample injection chamber. The mechanical pump was turned on to pump the sample to below 5 Pa, and the baffle valve was opened to send it into a sputtering chamber with a vacuum level (base vacuum) below 10⁻⁴ Pa. Multilayer composite electrodes and electrochromic layers were continuously deposited on the surface of the substrate by magnetron sputtering. ITO, Ag, and tungsten were used as targets. For the first transparent semiconductor, the sputtering gas was argon, the total pressure was 1 Pa, the distance between the target and the substrate was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 100 W, the sputtering time was 1 h, and the thickness was 400 nm. For the noble metal, the sputtering gas was argon, the total pressure was 0.6 Pa, the distance between the target and the substrate was 15 cm, the initial substrate temperature was room temperature, the DC power applied to the target was 20 W, the sputtering time was 2 min, and the thickness was 5 nm. The second transparent semiconductor uses argon as the sputtering gas, with a total pressure of 1 Pa, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 70 W applied to the target, a sputtering time of 10 min, and a thickness of 80 nm. Alternatively, using tungsten as the target, the sputtering gases are argon and oxygen, with a total pressure of 2.0 Pa, an oxygen partial pressure of 6%, a target-to-substrate distance of 15 cm, an initial substrate temperature of room temperature, a DC power of 70 W applied to the target or a power density of 1.54 W / cm², and a deposition time of 30 min, resulting in an inorganic electrochromic layer film with a thickness of approximately 350 nm.

[0121] (2) Prepare a 1 mol / L cationic salt solution, wherein the solvent is propylene carbonate and the solute is lithium perchlorate. Dissolve phenyltetracarboxylic dianhydride and hexylene diamine in the cationic salt solution and stir for 30 minutes to obtain a viscous polyamic acid solution, wherein the mass ratio of added monomer to cationic salt solution is 1:10, and the molar ratio of dianhydride monomer to diamine monomer is n:(n+1), n=50. Add triglycidyl-p-aminophenol, acetic anhydride and isoquinoline in the above amino-terminated polyamic acid solution in a ratio of 1:2%:1%:0.5% in sequence and stir for 10 minutes to obtain a mixed solution;

[0122] (3) Finally, the mixed solution was coated onto a flexible conductive substrate using a 20 μm wire rod and allowed to stand (50 °C for 1 h) to obtain a polyimide PC gel, which was then covered with an ITO transparent electrode. After the device cured, ethyl acetate was used to remove excess organic matter from the device surface. This resulted in an electrically driven broadband stealth system.

[0123] Table 1 shows the composition and fabrication of the electrically driven broadband stealth system:

[0124]

[0125] Table 2 shows the performance parameters of the electrically driven broadband stealth system:

[0126]

[0127]

Claims

1. An electrically driven broadband stealth system, characterized in that, It includes a substrate, a multilayer composite electrode, an electrochromic layer, a gel electrolyte layer, and a transparent electrode stacked sequentially; the multilayer composite electrode is composed of a first transparent semiconductor layer / a noble metal layer / a second transparent semiconductor layer; The gel electrolyte layer comprises a host material and a cationic salt distributed in the host material, wherein the host material is an amino-terminated polyimide resin; the molar ratio of the cationic salt to the amino-terminated polyimide resin is (2% to 5%):

1. The cationic salt is selected from at least one of Al salt, Li salt and Na salt; the thickness of the gel electrolyte layer is 10 to 100 μm.

2. The electrically driven broadband stealth system according to claim 1, characterized in that, The substrate is a silicon wafer substrate, a transparent glass substrate, or a metal substrate.

3. The electrically driven broadband stealth system according to claim 1, characterized in that, The first and second transparent semiconductor layers are made of materials independently selected from ITO, FTO and AZO; the noble metal layer is made of materials selected from at least one of Ag, Au, Pt and Pd.

4. The electrically driven broadband stealth system according to claim 1, characterized in that, The thickness of the first transparent semiconductor layer is 50–500 nm, the thickness of the noble metal layer is 1–10 nm, and the thickness of the second transparent semiconductor layer is 10–100 nm.

5. The electrically driven broadband stealth system according to claim 1, characterized in that, The electrochromic layer is made of WO3 material. 3-x The electrochromic layer contains at least one of V2O5, MoO3, Bruce Blue, and TiO2; the thickness of the electrochromic layer is 100–500 nm.

6. The electrically driven broadband stealth system according to claim 1, characterized in that, The transparent electrode is selected from at least one of transparent conductive oxides and metal nanowires; the surface sheet resistance of the transparent electrode is 10–40 Ω / cm. 2 Transmittance ≥75%.

7. The electrically driven broadband stealth system according to claim 1, characterized in that, The cation salt is selected from at least one of aluminum perchlorate, potassium perchlorate, and sodium perchlorate; The thickness of the gel electrolyte layer is 10–80 μm.

8. The electrically driven broadband stealth system according to claim 1, characterized in that, The method for preparing the gel electrolyte layer includes: (1) Dissolve the cationic salt in an organic solvent to obtain a cationic salt solution; (2) Add the dianhydride monomer and the diamine monomer to the cationic salt solution and mix to obtain an amino-terminated polyamic acid solution; (3) Add crosslinking agent, dehydrating agent and catalyst to amino-terminated polyamic acid solution and mix to obtain mixed solution; (4) The mixed solution is coated onto the substrate and left to stand at 30-80°C for 10 min to 2 h to obtain the gel electrolyte layer.

9. The electrically driven broadband stealth system according to claim 8, characterized in that, The organic solvent is at least one of propylene carbonate, diethyl carbonate (DEC), dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), and dimethyl glycol ether (DME). The concentration of the cation salt solution is 0.5–2 mol / L; The total mass ratio of the dianhydride monomer and the diamine monomer to the cationic salt solution is 1:(5-20). The molar ratio between the dianhydride monomer and the diamine monomer is n:(n+1), where n≥50; The dianhydride monomer is selected from at least one of pyromellitic dianhydride, benzophenone tetracarboxylic dianhydride, and diphenyl ether tetracarboxylic dianhydride, and the diamine monomer is selected from at least one of hexylene diamine, decylene diamine, diaminodiphenylmethane, diaminodiphenyl ether, p-phenylenediamine, m-phenylenediamine, m-toluene diamine, and diaminodiphenyl sulfone.

10. The electrically driven broadband stealth system according to claim 8, characterized in that, The crosslinking agent is selected from at least one of triglycidyl-p-aminophenol, triglycidyl-triisocyanate, tetraglycidyl-diaminodiphenylmethane, tetraglycidyl-diphenyldiamine, and pyromellitic acid chloride, and the amount added is 1% to 5% of the total mass of the amino-terminated polyamic acid solution; The dehydrating agent is selected from at least one of acetic anhydride, propionic anhydride, valeric anhydride, and dimethyl ketone, and the amount added is 0.5% to 5% of the total mass of the amino-terminated polyamic acid solution; The catalyst is selected from at least one of pyridine, 4-methylpyridine, 3,4-dimethylpyridine, isoquinoline, and triethylamine, and the amount added is 0.1% to 1% of the total mass of the amino-terminated polyamic acid solution.

11. The electrically driven broadband stealth system according to claim 1, characterized in that, An electric drive voltage is applied to an electrically driven broadband stealth system, which achieves at least three color variations and has an average emissivity of 0.1 to 0.8 in the near-infrared range of 780 nm to 2500 nm; the magnitude of the drive voltage is +2V to -4V.

Images