Ultrafast response hyperspectral electrochromic filter and preparation method thereof

Abstract

The invention relates to an ultrafast response hyperspectral electrochromic filter and a preparation method thereof. The ultrafast response hyperspectral electrochromic filter structurally comprises a glass substrate, a first transparent electrode, an electrolyte layer, an electrochromic layer, a second transparent electrode and a surface high-transmittance substrate which are sequentially stacked.

Description

Technical Field

[0001] The present invention belongs to the technical field of electrochromic functional materials and devices, and in particular relates to an ultrafast response hyperspectral electrochromic filter and a preparation method thereof. Background Art

[0002] 1-micron high-spectral band filters have many important applications in the field of communications, such as: (1) In the wavelength division multiplexing (WDM) system of optical fiber communication, 1-micron band filters can be used to implement wavelength division multiplexing and demultiplexing functions. In the WDM system, optical signals of different wavelengths are transmitted through the same optical fiber. The filter can accurately select and separate optical signals of specific wavelengths, thereby improving the bandwidth utilization of the optical fiber communication system; (2) It is used to shield noise signals in the fiber EDFA system and improve the signal-to-noise ratio and transmission quality of the signal; (3) In the radio-over-fiber (ROF) communication system of microwave photonics, 1-micron band filters can be used to process microwave carrier signals; (4) By transmitting microwave signals in optical fibers, low-loss signal transmission can be achieved, improving the performance of wireless communication systems; (5) Microwave photonic filters are used for filtering and processing microwave signals, which can achieve high-precision frequency selection and signal shaping, and are suitable for communication systems that require high-speed signal processing capabilities.

[0003] Currently, hyperspectral filters near 1 micron typically utilize thin-film, dielectric, and piezoelectric materials. Thin-film materials are typically composed of multiple dielectric layers, such as silicon dioxide (SiO2) and titanium dioxide (TiO2). However, they suffer from polarization dependence and temperature sensitivity. First, when light of different polarization states passes through a thin-film filter, its performance may vary, resulting in polarization-dependent loss (PDL). Second, thin-film filter performance may be affected by temperature fluctuations, leading to wavelength drift. Dielectric materials primarily include ceramics, such as rutile (TiO2). Disadvantages include complex manufacturing processes, requiring multiple steps such as tape casting and low-temperature stacking sintering, resulting in high costs. Ceramic dielectric materials also suffer from poor temperature stability and susceptibility to temperature drift. Piezoelectric materials primarily include aluminum nitride (AlN) and other piezoelectric materials. Disadvantages include difficulty in fabrication. High-quality piezoelectric thin films require precise control of parameters such as deposition temperature and gas concentration, resulting in high process requirements. Furthermore, compatibility with integrated circuit processes is poor, as excessively high deposition temperatures may be incompatible with integrated circuit processes. Summary of the Invention

[0004] In view of the above technical problems, the object of the present invention is to provide an ultrafast response hyperspectral electrochromic filter and a preparation method thereof.

[0005] In a first aspect, the present invention provides an ultrafast response hyperspectral electrochromic filter, the structure of which includes: a glass substrate, a first transparent electrode, an electrolyte layer, an electrochromic layer, a second transparent electrode and a surface high-transmittance substrate stacked in sequence.

[0006] Preferably, the material of the first transparent electrode and the second transparent electrode includes at least one of transparent conductive oxide, MXENE, and metal nanowires, preferably ITO indium tin oxide; the sheet resistance is 10 to 400 Ω / cm 2 , the transmittance in the 0.7-1.3um hyperspectral band is ≥85%, and the transmittance in the 0.38-2.5μm band of sunlight is ≥75%.

[0007] Preferably, the electrolyte layer is a cationic gel conductive layer based on organic resin, and the cations include Li + 、Al 3+ , K + and Na + At least one of; preferably, the thickness of the electrolyte layer is 10-50 μm.

[0008] Preferably, the material of the electrochromic layer includes WO 3-x 、MoO 3-x 、TiO 2-x and at least one of polythiophene, polypyrrole, polyaniline and Prussian blue; the thickness is 200-600 nm; the refractive index n value in the 0.7-1.3 μm high spectral range satisfies 1.97≤n≤1.98, and the extinction coefficient is 0.0001≤k≤0.00012.

[0009] In a second aspect, the present invention provides a method for preparing the above-mentioned ultrafast response hyperspectral electrochromic filter, the preparation method comprising the following steps: (1) A first transparent electrode is prepared on the surface of a glass substrate by magnetron sputtering, and a second transparent electrode and an electrochromic layer are sequentially prepared on the surface of a high-transmittance substrate; (2) Filling the electrolyte solution between the electrochromic layer and the first transparent electrode through a vacuum drip irrigation process and curing the electrolyte solution to obtain the ultrafast response hyperspectral electrochromic filter.

[0010] Preferably, in step (1), the method for preparing the electrochromic layer on the second transparent electrode includes magnetron sputtering, spin coating or electrodeposition; wherein, the process parameters for preparing the electrochromic layer by magnetron sputtering include: using metal tungsten, molybdenum or titanium as the target material, the sputtering gas is argon and oxygen, the total pressure is 0.5-2.0 Pa, the oxygen partial pressure is 0-50%, the distance between the target material and the substrate is 10-20 cm, the initial substrate temperature is room temperature, the DC power applied to the target material is 30-150 W or the power density is 0.6-3.0 W / cm 2 .

[0011] Preferably, step (1) further includes heat treatment of the electrochromic layer after it is formed by magnetron sputtering; wherein the heat treatment is carried out in an oxygen environment and under normal pressure, and the specific process includes: heating to 300-400°C for 10-60s and then keeping warm for 10-100s, then heating to 350-500°C for 5-60s and then keeping warm for 100-1000s, and naturally cooling to room temperature.

[0012] Preferably, in step (2), the preparation method of the electrolyte solution comprises: weighing a photocurable resin, a solvent, a co-solvent, ferrocene, ETPTA and an ion source solution in a mass ratio of 1: (1-3): (0.5-2): (0.05-0.2): (0.5-2): (1-3), mixing, adding 0.1-0.5% of an initiator and mixing again to obtain the electrolyte solution.

[0013] Preferably, the photocurable resin is Xianmet UC935, the solvent is PMA propylene glycol methyl ether acetate, the co-solvent is PFPN ethoxypentafluorocyclotriphosphazene, and the initiator is initiator 1173.

[0014] Preferably, the ion source in the ion source solution includes at least one of chlorides, perchlorates and sulfates of Li, Na, Mg or Zn, and the solvent includes at least one of propylene carbonate, ethylene carbonate and ethylpropyl carbonate; preferably, the concentration of the ion source solution is 0.1-2 mol / L.

[0015] Beneficial effects (1) The present invention introduces an appropriate amount of weak polar cosolvent into the electrolyte, which can weaken the Li + The interaction between cations and solvent molecules such as PC accelerates the desolvation of cations and improves ionic conductivity; at the same time, it can also reduce the interaction between solvent molecules such as PC and ClO in the ion source. 4-The interaction between the anions reduces the decomposition of solvent molecules such as PC, improves the wide voltage stability of the electrolyte layer, and improves the response speed and cycle stability of the electrochromic filter. In addition, there is an interaction force between the weak polar co-solvents such as PFPN and the solvent molecules such as PC, which will destroy the network formed between the solvent molecules such as PC-PC, stabilize the solvent molecules such as PC, and reduce the possibility of PC decomposition or coordination. (2) The present invention further enhances the selectivity and regulation capability at 1 μm wavelength in the device, and through structural innovation, it has obvious preferential regulation capability for the hyperspectral band near 1 μm, thus being applicable to hyperspectral filters; (3) With respect to the application of filters, the present invention significantly improves the response speed of electrochromic filters through material innovation. The designed electrochromic device has excellent selective control performance for high spectrum through structural and material innovation. The adjustment amplitude can be controlled and selected according to the size of the external field voltage drive. Moreover, the electrochromic filter designed by the present invention is used in conjunction with a photoelectric sensor, which can dynamically control filtering and adapt to a richer range of application scenarios. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 This is a schematic diagram of an exemplary structure of the ultrafast response hyperspectral electrochromic filter provided by the present invention. DETAILED DESCRIPTION

[0017] The present invention is further described below through the following embodiments. It should be understood that the following embodiments are only used to illustrate the present invention, rather than to limit the present invention.

[0018] First, if Figure 1 As shown, the present invention provides an ultrafast response hyperspectral electrochromic filter. The structure of the ultrafast response hyperspectral electrochromic filter may include: a glass substrate, a first transparent electrode, an electrolyte layer, an electrochromic layer, a second transparent electrode, and a surface high-transmittance substrate stacked in sequence.

[0019] In some embodiments, the glass substrate may have a thickness of 0.05-2 mm.

[0020] In some embodiments, the material of the first transparent electrode and the second transparent electrode may include at least one of transparent conductive oxide, MXENE, and metal nanowires, preferably ITO indium tin oxide; the sheet resistance may be 10 to 400 Ω / cm 2 , the transmittance in the 0.7-1.3um hyperspectral band is ≥85%, and the transmittance in the 0.38-2.5μm band of sunlight is ≥75%.

[0021] In some embodiments, the electrolyte layer may be a cationic gel conductive layer based on an organic resin, and the cations may include Li+ 、Al 3+ , K + and Na + At least one of; preferably, the thickness of the electrolyte layer can be 10-50 μm.

[0022] In some embodiments, the material of the electrochromic layer may include WO 3-x 、MoO 3-x 、TiO 2-x and at least one of polythiophene, polypyrrole, polyaniline and Prussian blue; the thickness can be 200-600 nm; the refractive index n value in the 0.7-1.3 μm high spectral range satisfies 1.97≤n≤1.98, and the extinction coefficient is 0.0001≤k≤0.00012.

[0023] In some embodiments, the material of the high-transmittance surface substrate may include one of glass, polymethyl methacrylate (PMMA), and polycarbonate (PC).

[0024] In some embodiments, the response speed of the ultrafast response hyperspectral electrochromic filter is ≤2s, the response capability when the external field driving voltage is 0.5V is ≥20%, the response capability when the external field driving voltage is 1V is ≥40%, the response capability when the external field driving voltage is 2V is ≥60%, the number of cycles is ≥20,000 times, and the temperature volatility is ≤2%; wherein, the temperature volatility refers to the change in the ability to adjust the hyperspectral band at the same voltage from 10°C to 80°C.

[0025] Typically, the filtering capacity of a hyperspectral filter is static and unadjustable. The electrochromic filter disclosed in the present invention exhibits excellent hyperspectral selectivity and controllability, and can also selectively adjust its amplitude based on the magnitude of the external field voltage drive. In other words, through innovative structural and material design, the present invention not only improves the response speed of the hyperspectral filter but also significantly enhances its hyperspectral filtering capability, specifically its ability to adjust wavelengths around 1 micron. Therefore, the electrochromic filter designed in the present invention, when used in conjunction with a photoelectric sensor, enables dynamic and controllable filtering, adapting to a wider range of application scenarios.

[0026] It should be noted that the present invention heat treats the electrochromic layer such as WO3 in the device to regulate the proportion and distribution of its oxygen vacancies, and simultaneously uses oxidation air to regulate the generation of local surface plasmon resonance (LSPR), ultimately producing strong plasma resonance absorption of the hyperspectral band around 1 μm. In other words, the surface plasmon resonance absorption position is adjusted to around 1 μm, giving it the best regulation capability around 1 μm. Moreover, through structural innovation, the present invention allows the electrochromic layer such as WO3 in the device to be regarded as a transparent layer in the resonant cavity, giving it a significant preferential regulation capability for the hyperspectral band around 1 μm, and thus can be applied to hyperspectral filters. For filter applications, this patent significantly improves the response speed of electrochromic filters through material innovation.

[0027] The following is an exemplary description of the method for preparing the ultrafast response hyperspectral electrochromic filter provided by the present invention. The preparation method may include the following steps: (1) A first transparent electrode is prepared on the surface of a glass substrate by magnetron sputtering, and a second transparent electrode and an electrochromic layer are sequentially prepared on the surface of a high-transmittance substrate; (2) Filling the electrolyte solution between the electrochromic layer and the first transparent electrode through a vacuum drip irrigation process and curing the electrolyte solution to obtain the ultrafast response hyperspectral electrochromic filter.

[0028] In some embodiments, in step (1), the method for preparing the electrochromic layer on the second transparent electrode may include magnetron sputtering, spin coating or electrodeposition; wherein, the process parameters for preparing the electrochromic layer by magnetron sputtering may include: using metal tungsten, molybdenum or titanium as the target material, the sputtering gas is argon and oxygen, the total pressure is 0.5-2.0 Pa, the oxygen partial pressure is 0-50%, the distance between the target material and the substrate is 10-20 cm, the initial substrate temperature is room temperature, and the DC power applied to the target material is 30-150 W or the power density is 0.6-3.0 W / cm 2 .

[0029] In some embodiments, step (1) further includes heat treatment of the electrochromic layer after magnetron sputtering forms the electrochromic layer; wherein the heat treatment can be carried out in an oxygen environment and at normal pressure, and the specific process may include: heating to 300-400°C for 10-60s and then keeping the temperature for 10-100s, then heating to 350-500°C for 5-60s and then keeping the temperature for 100-1000s, and naturally cooling to room temperature. As an example, the temperature can be raised to 350°C for 20s, kept at this temperature for 30s, then raised to 450°C for 10s, kept at this temperature for 300s, and naturally cooled to room temperature. By adopting rapid thermal treatment, the refractive index and extinction coefficient of the electrochromic layer in the hyperspectral band can be adjusted. In addition, by limiting the parameters related to the thermal treatment, the surface oxygen vacancy concentration, that is, the surface electron concentration, which is closely related to the resonant absorption peak of the LSPR, can be adjusted. If the holding time is too long, the oxygen vacancy content will be too low, and the LSPR resonance absorption capacity will be insufficient; if the holding time is too short, the oxygen vacancy content will be too high, and the control range will be between 1.2-1.5um (non-hyperspectral range).

[0030] To be more specific, the DC magnetron sputtering system equipment used in the magnetron sputtering deposition of the present invention may include a deposition chamber, a sampling chamber, several target heads, a substrate plate, a DC current and a series of mechanical pumps and vacuum pumps, wherein the target head and the substrate plate are at a certain angle and a certain distance apart, and the DC power supply is connected to the target head. The substrate is ultrasonically cleaned, and the substrate is ultrasonically cleaned with acetone, anhydrous ethanol, and deionized water for 20 minutes each, and blown dry with compressed air. Cover a certain part of the conductive substrate with high-temperature tape as an electrode, and fix it on the substrate tray, put it into the sampling chamber, turn on the mechanical pump to pump it below 5Pa, and then open the baffle valve to send it into the vacuum degree (background vacuum degree) that has reached 10 -4 Pa and below in the sputtering room.

[0031] The specific sputtering deposition process is as follows: high-purity argon and oxygen gas are introduced into the sputtering chamber, with the purity of the argon and oxygen used being 99.99% or higher. The total pressure and oxygen partial pressure in the chamber are controlled within the ranges of 0.5-2.0 Pa and 0-50%, respectively, with the oxygen partial pressure preferably being 0-25%. The vertical distance between the target and the substrate is controlled to be 10-20 cm, and the initial substrate temperature is room temperature. The DC power supply is turned on and the power is controlled to be 30-200 W. The pre-sputtering time is 5-30 minutes, the sputtering time is 10-60 minutes, and the substrate temperature is room temperature. After the sputtering is completed, the substrate is removed after the substrate temperature cools to room temperature.

[0032] In some embodiments, in step (2), the method for preparing the electrolyte solution may include: weighing a photocurable resin, a solvent, a co-solvent, ferrocene, ethoxylated trimethylolpropane triacrylate ETPTA, and an ion source solution in a mass ratio of 1: (1-3): (0.5-2): (0.05-0.2): (0.5-2): (1-3), mixing, adding 0.1-0.5% of an initiator, and mixing again to obtain the electrolyte solution.

[0033] The photocurable resin may be Xianmeite UC935, the solvent may be PMA propylene glycol methyl ether acetate, the co-solvent may be PFPN ethoxypentafluorocyclotriphosphazene, and the initiator may be initiator 1173.

[0034] The ion source in the ion source solution may include at least one of chlorides, perchlorates and sulfates of Li, Na, Mg or Zn, and the solvent may include at least one of propylene carbonate (PC), ethylene carbonate (EC) and ethyl propyl carbonate (EMC); preferably, the concentration of the ion source solution may be 0.1-2 mol / L.

[0035] It should be noted that the present invention introduces an appropriate amount of weak polar cosolvent into the electrolyte, which can weaken the Li + The interaction between cations and solvent molecules such as PC accelerates the desolvation of cations and improves ionic conductivity; at the same time, it can also reduce the interaction between solvent molecules such as PC and ClO in the ion source. 4- The interaction between PFPN and anions reduces the decomposition of solvent molecules such as PC, improving the wide-voltage stability of the electrolyte layer and enhancing the response speed and cycling stability of the electrochromic filter. Furthermore, the interaction between weakly polar cosolvents such as PFPN and solvent molecules such as PC disrupts the network formed between PC-PC solvent molecules, stabilizing PC and other solvent molecules and reducing the possibility of PC decomposition or coordination. The addition of PFPN disrupts the solvation environment of ions in the electrolyte, thereby improving the response speed of the device.

[0036] In some embodiments, in step (2), the curing method can be ultraviolet curing (such as 100W) or thermal curing.

[0037] The preparation process of the invention is simple, low in cost and easy to promote. The ultrafast response high-spectral electrochromic filter developed by the invention has a broader application prospect.

[0038] The following examples are further given to illustrate the present invention in detail. It should be understood that the following examples are only used to further illustrate the present invention and cannot be interpreted as limiting the scope of protection of the present invention. Some non-essential improvements and adjustments made by those skilled in the art based on the above content of the present invention all fall within the scope of protection of the present invention. The specific process parameters and the like in the following examples are only examples within a suitable range, and those skilled in the art can make selections within a suitable range through the description herein, and are not limited to the specific numerical values ​​exemplified below. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.

[0039] Example 1

[0040] The method for preparing the ultrafast response hyperspectral electrochromic filter provided in this embodiment includes the following steps: (1) Magnetron sputtering is used to prepare a first transparent electrode on the surface of a glass substrate, and a second transparent electrode and an electrochromic layer are prepared in sequence on the surface of a high-transmittance substrate; high-spectral and high-transmittance ITO is used as the first transparent electrode and the second transparent electrode; the process of preparing the electrochromic layer by magnetron sputtering may include: using metal tungsten, molybdenum or titanium as a 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 and the substrate 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 1.4 W / cm 2 A 400nm thick electrochromic layer was deposited on the surface using a DC power supply. Subsequently, the device was heat treated in an oxygen environment at atmospheric pressure, heating to 350°C for 20 seconds, holding for 30 seconds, heating to 450°C for 10 seconds, holding for 300 seconds, and then naturally cooling to room temperature. (2) According to the existing technology, an electrolyte solution prepared by weighing a photocurable resin (Xianmeite UC935), a solvent (PMA propylene glycol methyl ether acetate), a co-solvent PFPN, ferrocene, ETPTA and a lithium ion source solution in a mass ratio of 1:2:1:0.1:1:2 is filled between the above-mentioned electrochromic layer and the first transparent electrode by vacuum drip irrigation; wherein the ion source in the ion source solution is selected as Li perchlorate, the solvent is propylene carbonate, and the concentration range of the ion source solution is 1 mol / L; a complete device is formed by ultraviolet curing or thermal curing; the thickness of the resin layer is controlled to be 20 μm by the surface tension of the hard template and the resin solution; wherein, the photocuring is to place the device under a 100W ultraviolet lamp for uniform irradiation; after the device is cured, an organic solvent is used to remove excess organic matter on the surface of the device to obtain the ultrafast response hyperspectral electrochromic filter.

[0041] Example 2

[0042] The preparation method of the ultrafast response hyperspectral electrochromic filter provided in this embodiment refers to that in Example 1, with the following main differences: In step (1), the thickness of the electrochromic layer is 200 nm.

[0043] Example 3

[0044] The preparation method of the ultrafast response hyperspectral electrochromic filter provided in this embodiment refers to that in Example 1, with the following main differences: In step (1), the thickness of the electrochromic layer is 600 nm.

[0045] Example 4

[0046] The preparation method of the ultrafast response hyperspectral electrochromic filter provided in this embodiment refers to that in Example 1, with the following main differences: In step (2), the mass ratio of the raw materials of the electrolyte solution is 1:2:0.5:0.1:1:2.

[0047] Example 5

[0048] The preparation method of the ultrafast response hyperspectral electrochromic filter provided in this embodiment refers to that in Example 1, with the following main differences: In step (2), the mass ratio of the raw materials of the electrolyte solution is 1:2:2:0.1:1:2.

[0049] Example 6

[0050] The preparation method of the ultrafast response hyperspectral electrochromic filter provided in this embodiment refers to that in Example 1, with the following main differences: In step (2), the thickness of the resin layer is controlled to be 10 μm by the surface tension of the hard template and the resin solution.

[0051] Example 7

[0052] The preparation method of the ultrafast response hyperspectral electrochromic filter provided in this embodiment refers to that in Example 1, with the following main differences: In step (2), the thickness of the resin layer is controlled to be 50 μm by the surface tension of the hard template and the resin solution.

[0053] Example 8

[0054] The preparation method of the ultrafast response hyperspectral electrochromic filter provided in this embodiment refers to that in Example 1, with the following main differences: In step (1), the process for heat treatment of the electrochromic film deposited by magnetron sputtering is as follows: in an oxygen environment, at normal pressure, heating to 350°C for 20 seconds, keeping warm for 100 seconds, heating to 450°C for 10 seconds, keeping warm for 200 seconds, and naturally cooling to room temperature.

[0055] Example 9

[0056] The preparation method of the ultrafast response hyperspectral electrochromic filter provided in this embodiment refers to that in Example 1, with the following main differences: In step (1), the process for heat treatment of the electrochromic film after magnetron sputtering deposition is: in an oxygen environment, at normal pressure, heating to 350°C for 20s, keeping warm for 10s, heating to 450°C for 10s, keeping warm for 300s, and naturally cooling to room temperature.

[0057] Example 10

[0058] The preparation method of the ultrafast response hyperspectral electrochromic filter provided in this embodiment refers to that in Example 1, with the following main differences: In step (1), the process of heat treatment of the electrochromic film after magnetron sputtering deposition is as follows: in an oxygen environment, at normal pressure, heating to 350°C for 60s, keeping warm for 30s, heating to 450°C for 10s, keeping warm for 300s, and naturally cooling to room temperature.

[0059] Example 11

[0060] The preparation method of the ultrafast response hyperspectral electrochromic filter provided in this embodiment refers to that in Example 1, with the following main differences: In step (1), the process for heat treatment of the electrochromic film after magnetron sputtering deposition is: in an oxygen environment, at normal pressure, heating to 350°C for 20s, keeping warm for 30s, heating to 450°C for 60s, keeping warm for 300s, and naturally cooling to room temperature.

[0061] Comparative Example 1

[0062] The preparation method of the electrochromic filter provided in this comparative example refers to that in Example 1, with the main differences being: In step (2), no co-solvent PFPN is added to the electrolyte solution.

[0063] Comparative Example 2

[0064] The preparation method of the electrochromic filter provided in this comparative example refers to that in Example 1, with the main differences being: In step (2), the mass ratio of the raw materials of the electrolyte solution is 1:2:3:0.1:1:2.

[0065] Comparative Example 3

[0066] The preparation method of the electrochromic filter provided in this comparative example refers to that in Example 1, with the main differences being: In step (1), the process of heat treating the electrochromic film deposited by magnetron sputtering is as follows: in an oxygen environment, at normal pressure, heating to 350° C. in 20 seconds, keeping the temperature for 300 seconds, and naturally cooling to room temperature.

[0067] Comparative Example 4

[0068] The preparation method of the electrochromic filter provided in this comparative example refers to that in Example 1, with the main differences being: In step (1), the process of heat treating the electrochromic film deposited by magnetron sputtering is as follows: in an oxygen environment, at normal pressure, heating to 450° C. for 20 seconds, keeping the temperature for 300 seconds, and naturally cooling to room temperature.

[0069] Table 1 below shows the relevant parameters of the electrochromic filters prepared in Examples 1-11 and Comparative Examples 1-4:

[0070] Although the present invention has been described in detail through the above preferred embodiments, it should be understood that the above description is not intended to limit the present invention. After reading the above description, various modifications and substitutions of the present invention will become apparent to those skilled in the art. Therefore, the scope of protection of the present invention should be defined by the appended claims.

Claims

1. An ultrafast response hyperspectral electrochromic filter, characterized in that: The structure of the ultrafast response hyperspectral electrochromic filter comprises: a glass substrate, a first transparent electrode, an electrolyte layer, an electrochromic layer, a second transparent electrode and a surface high-transmittance substrate stacked in sequence.

2. The ultrafast response hyperspectral electrochromic filter according to claim 1, characterized in that: The material of the first transparent electrode and the second transparent electrode includes at least one of transparent conductive oxide, MXENE, and metal nanowires, preferably ITO indium tin oxide; the sheet resistance is 10 to 400 Ω / cm 2 , the transmittance in the 0.7-1.3um hyperspectral band is ≥85%, and the transmittance in the 0.38-2.5μm band of sunlight is ≥75%.

3. The ultrafast response hyperspectral electrochromic filter according to claim 1 or 2, characterized in that: The electrolyte layer is a cationic gel conductive layer based on organic resin, and the cations include Li + 、Al 3+ , K + and Na + At least one of; preferably, the thickness of the electrolyte layer is 10-50 μm.

4. The ultrafast response hyperspectral electrochromic filter according to any one of claims 1 to 3, characterized in that: The material of the electrochromic layer includes WO 3-x 、MoO 3-x 、TiO 2-x and at least one of polythiophene, polypyrrole, polyaniline and Prussian blue; the thickness is 200-600 nm; the refractive index n value in the 0.7-1.3 μm high spectral range satisfies 1.97≤n≤1.98, and the extinction coefficient is 0.0001≤k≤0.00012.

5. A method for preparing an ultrafast response hyperspectral electrochromic filter according to any one of claims 1 to 4, characterized in that: The preparation method comprises the following steps: (1) A first transparent electrode is prepared on the surface of a glass substrate by magnetron sputtering, and a second transparent electrode and an electrochromic layer are sequentially prepared on the surface of a high-transmittance substrate; (2) Filling the electrolyte solution between the electrochromic layer and the first transparent electrode through a vacuum drip irrigation process and curing the electrolyte solution to obtain the ultrafast response hyperspectral electrochromic filter.

6. The preparation method according to claim 5, characterized in that In step (1), the method for preparing the electrochromic layer on the second transparent electrode includes magnetron sputtering, spin coating or electrodeposition; wherein, the process parameters for preparing the electrochromic layer by magnetron sputtering include: using metal tungsten, molybdenum or titanium as the target material, the sputtering gas is argon and oxygen, the total pressure is 0.5-2.0 Pa, the oxygen partial pressure is 0-50%, the distance between the target material and the substrate is 10-20 cm, the initial substrate temperature is room temperature, and the DC power applied to the target material is 30-150 W or the power density is 0.6-3.0 W / cm 2 .

7. The preparation method according to claim 5 or 6, characterized in that: Step (1) further includes heat treatment of the electrochromic layer after it is formed by magnetron sputtering; wherein the heat treatment is carried out in an oxygen environment and under normal pressure, and the specific process includes: heating to 300-400°C for 10-60s and then keeping warm for 10-100s, then heating to 350-500°C for 5-60s and then keeping warm for 100-1000s, and naturally cooling to room temperature.

8. The preparation method according to any one of claims 5 to 7, characterized in that In step (2), the preparation method of the electrolyte solution includes: weighing a photocurable resin, a solvent, a co-solvent, ferrocene, ETPTA and an ion source solution in a mass ratio of 1: (1-3): (0.5-2): (0.05-0.2): (0.5-2): (1-3), mixing, adding 0.1-0.5% of an initiator and mixing again to obtain the electrolyte solution.

9. The preparation method according to any one of claims 5 to 8, characterized in that The photocurable resin is Xianmeite UC935, the solvent is PMA propylene glycol methyl ether acetate, the co-solvent is PFPN ethoxy pentafluorocyclotriphosphazene, and the initiator is initiator 1173.

10. The preparation method according to any one of claims 5 to 9, characterized in that: The ion source in the ion source solution includes at least one of chlorides, perchlorates and sulfates of Li, Na, Mg or Zn, and the solvent includes at least one of propylene carbonate, ethylene carbonate and ethylpropyl carbonate; preferably, the concentration of the ion source solution is 0.1-2 mol / L.

Images