Electrochromic glass and method of making and using the same

Abstract

The application relates to an electrochromic glass and a preparation method and application thereof, the electrochromic glass comprising a glass substrate, a first conductive layer arranged on the glass substrate, a laser groove arranged on the first conductive layer, a first electrode, an insulating layer and an electrochromic layer arranged on the first conductive layer in sequence, a second conductive layer arranged on the electrochromic layer, a protective layer and a second electrode arranged on the second conductive layer in sequence, and a protective layer arranged on the second electrode layer. The application directly prepares the electrode on the first conductive layer, reduces the process flow, and increases the insulating layer (the spacer) to isolate the upper and lower conductive layers and prevent the occurrence of electrode short circuit.

Description

TECHNICAL FIELD

[0001] The present application relates to an electrochromic glass and its preparation method and application, belonging to the field of electrochromic materials. BACKGROUND

[0002] In order to form a conductive path for the electrochromic coating layer, electrodes for connecting the first conductive layer and the second conductive layer are distributed on the electrochromic glass, also known as conductive bus bars or simply bus bars. In order to realize the bus bar, laser scribing is generally used at present, such as the prior art discloses at least 4 times of laser scribing to form the bus bar. Under this process condition, the increase of the scribing process greatly reduces the qualified rate. In addition, the scribing process requires extremely high laser equipment, such as the thinnest film layer for scribing is only about 100 nm, which requires the control accuracy of laser energy to be more than ±0.01%, and a large energy deviation easily leads to the fact that the film layer cannot be scribed through or the film layer is damaged, and causes a large resistance value, forms a hot spot, and affects the color changing effect. At the same time, the laser platform requires extremely high flatness, and the flatness of the platform directly affects the laser focal point and the scribing effect. SUMMARY

[0003] Therefore, the main purpose of the present application is to provide an electrochromic glass and its preparation method and application, and the technical problem to be solved is to prevent the occurrence of electrode short circuit by increasing the insulation layer to isolate the upper and lower conductive layers.

[0004] The purpose of the present application and the technical problem thereof are realized by adopting the following technical scheme. The present application provides an electrochromic glass, which comprises a glass substrate, a first conductive layer is arranged on the glass substrate, the first conductive layer has a laser groove, a first electrode layer, an insulation layer and an electrochromic layer are sequentially arranged on the first conductive layer, a second conductive layer is arranged on the electrochromic layer, a protective layer and a second electrode layer are sequentially arranged on the second conductive layer, and a protective layer is arranged on the second electrode layer.

[0005] Preferably, in the aforementioned electrochromic glass, protective layers are arranged on the first electrode layer and the insulation layer.

[0006] Preferably, in the aforementioned electrochromic glass, the electrochromic layer is located above the laser groove.

[0007] Preferably, in the aforementioned electrochromic glass, the first conductive layer or the second conductive layer is selected from one of an indium tin oxide layer, a fluorine tin oxide layer and an aluminum-doped zinc oxide graphene layer.

[0008] Preferably, in the aforementioned electrochromic glass, the thickness of the first conductive layer or the second conductive layer is 200 nm-350 nm.

[0009] Preferably, in the aforementioned electrochromic glass, the number of scribe lines of the laser grooves is 5-50; the width of the laser grooves is 0.02mm-0.2mm; and the depth of the laser grooves is 200nm-500nm.

[0010] Preferably, in the aforementioned electrochromic glass, the width of the first electrode layer or the second electrode layer is 1mm-30mm, and the resistance is 5-12Ω / km.

[0011] Preferably, in the aforementioned electrochromic glass, the first electrode layer comprises a plurality of first electrodes, each having a width of 0.02mm-2mm and a thickness of 200nm-500nm; the second electrode layer comprises a plurality of second electrodes, each having a width of 0.02mm-2mm and a thickness of 200nm-500nm; and the material of the first electrode or the second electrode is selected from conductive silver paste, indium and its alloys, or tin and its alloys.

[0012] Preferably, in the aforementioned electrochromic glass, the insulating layer is selected from thermosetting materials or ultraviolet curing materials.

[0013] Preferably, in the aforementioned electrochromic glass, the width of the insulating layer is 0.1mm-20mm.

[0014] Preferably, in the aforementioned electrochromic glass, the electrochromic layer comprises, in sequence, a tungsten oxide film, a lithium oxide film, and a nickel-tungsten oxide film deposited on the first conductive layer; the thickness of the tungsten oxide film is 120nm-130nm; the thickness of the lithium oxide film is 200nm-350nm; and the thickness of the nickel-tungsten oxide film is 65nm-80nm.

[0015] Preferably, in the aforementioned electrochromic glass, the protective layer is silicon aluminum oxide, silicon oxide, niobium oxide, titanium oxide, or zirconium oxide, and has a thickness of 170nm-220nm.

[0016] The purposes and technical problems of the present application can also be further achieved by the following technical measures. The present application provides a preparation method of an electrochromic glass, comprising the following steps:

[0017] First glass cleaning;

[0018] Deposition of a first conductive layer;

[0019] Laser scribing of the first conductive layer;

[0020] Preparation of an insulating layer on the first conductive layer;

[0021] Preparation of a first electrode;

[0022] Deposition of an electrochromic layer;

[0023] Deposit a second conductive layer;

[0024] A second electrode is fabricated on the second conductive layer;

[0025] Deposition protective layer.

[0026] Preferably, in the aforementioned method for preparing electrochromic glass, the preparation of the first conductive layer specifically includes the following steps: vacuum reactive magnetron sputtering deposition, using an ITO target, argon gas at 400 sccm, vacuum degree at 0.3 Pa-0.6 Pa, deposition temperature at 200℃-250℃, power at 9 kW for at least 5 min of target burning, oxygen flow at 7 sccm-9 sccm, and after the voltage and current stabilize, glass deposition begins at a deposition speed of 0.1 m / min-1 m / min, holding at 200℃-250℃ for 20 min-60 min to complete the preparation of the first conductive layer, with a thickness of 200 nm-350 nm.

[0027] Preferably, in the aforementioned method for preparing electrochromic glass, the laser scribing of the first conductive layer specifically includes the following steps: laser scribing on the first conductive layer.

[0028] Preferably, in the aforementioned method for preparing electrochromic glass, the laser used for laser scribing the first conductive layer is an infrared laser, a green laser, an ultraviolet laser, or a picosecond laser.

[0029] Preferably, in the aforementioned method for preparing electrochromic glass, the preparation of an insulating layer on the first conductive layer specifically includes the following steps: applying insulating material onto the first conductive layer, followed by air cooling to form the insulating layer.

[0030] Preferably, in the aforementioned method for preparing electrochromic glass, the preparation of an insulating layer on the first conductive layer specifically includes the following steps: placing an insulating material on the surface of the first conductive layer, then applying pressure to the insulating material on both sides of the first conductive layer, and making it come into close contact with the conductive layer by local heating.

[0031] Preferably, in the aforementioned method for preparing electrochromic glass, the preparation of the first electrode layer specifically includes the following steps: taking 30ml-50ml of conductive silver paste and adding it to a dispensing device, setting the dispensing focus and dispensing position, the dispensing width being 0.02mm-2mm and the thickness being 200-500nm, and after dispensing, using a curing cabinet to heat and dry at 120℃-350℃ to complete the preparation of the first electrode layer.

[0032] Preferably, in the aforementioned method for preparing electrochromic glass, the preparation of the electrochromic layer specifically includes the following steps: The electrochromic layer is prepared using reactive magnetron sputtering. First, a tungsten oxide thin film is prepared on the first conductive layer using a magnetron sputtering tungsten target. Argon gas is introduced into the vacuum chamber, controlling the argon flow rate to be 40 sccm-50 sccm and the oxygen flow rate to be 60 sccm-70 sccm, maintaining the working pressure at 0.6 Pa-0.65 Pa, and the thickness of the tungsten oxide thin film to be 120 nm-130 nm. Subsequently, a lithium oxide thin film is prepared on the surface of the tungsten oxide thin film using a magnetron sputtering lithium oxide target, and argon gas is introduced into the vacuum chamber. The flow rate of argon gas is controlled at 15 sccm-20 sccm, and the working pressure is maintained at 0.4 Pa-0.45 Pa. The thickness of the lithium oxide film is 200 nm-350 nm. Then, a nickel-tungsten oxide film is prepared on the surface of the lithium oxide film using a magnetron sputtering nickel target. Argon gas is introduced into the vacuum chamber, and the flow rate of argon gas is controlled at 40 sccm-50 sccm, the flow rate of oxygen is controlled at 100 sccm-120 sccm, and the working pressure is maintained at 0.6 Pa-0.7 Pa. The thickness of the nickel-tungsten oxide film is 65 nm-80 nm. The total thickness of the electrochromic layer is 380 nm-600 nm.

[0033] Preferably, in the aforementioned method for preparing electrochromic glass, the preparation of the second conductive layer specifically includes the following steps: vacuum reactive magnetron sputtering deposition, using an ITO target, argon gas at 400 sccm, vacuum degree at 0.3 Pa-0.6 Pa, deposition temperature at 200℃-250℃, power at 9 kW for at least 5 min of target burning, oxygen flow at 7 sccm-9 sccm, and after the voltage and current stabilize, glass deposition begins at a deposition speed of 0.1 m / min-1 m / min, holding at 200℃-250℃ for 20 min-60 min to complete the preparation of the second conductive layer, with a thickness of 200 nm-350 nm.

[0034] Preferably, in the aforementioned method for preparing electrochromic glass, the preparation of the second electrode layer on the second conductive layer specifically includes the following steps: taking 30ml-50ml of conductive silver paste and adding it to the dispensing equipment, setting the dispensing focus and dispensing position, the dispensing width being 0.02mm-2mm, and the thickness being 200nm-500nm. After dispensing, the second electrode layer is prepared by heating and drying in a curing cabinet at 120℃-350℃.

[0035] Preferably, in the aforementioned method for preparing electrochromic glass, the deposition of the protective layer specifically includes the following steps: vacuum reactive magnetron sputtering deposition is performed using a silicon target. Argon gas at 600 sccm-700 sccm is introduced, and a power of 9 KW-11 KW is used to first burn the target. Then, oxygen gas at 300 sccm-350 sccm is introduced. After the current and voltage stabilize, the deposition begins, and the thickness is 170 nm-220 nm, thus completing the preparation of the protective layer.

[0036] The objectives of this invention and the technical problems it addresses can be further achieved by the following technical measures.

[0037] The present invention proposes a building curtain wall, which includes the aforementioned electrochromic glass.

[0038] The objectives of this invention and the technical problems it addresses can be further achieved by the following technical measures.

[0039] The present invention proposes an exterior window, the exterior window comprising actively adjustable energy-saving glass, the actively adjustable energy-saving glass comprising the aforementioned electrochromic glass.

[0040] By employing the above technical solutions, the electrochromic glass, its preparation method, and its applications provided by the present invention have at least the following advantages:

[0041] This invention reduces the process steps by directly fabricating electrodes on the first conductive layer; it adds an insulating layer (isolation material) to isolate the upper and lower conductive layers, preventing short circuits in the electrodes. This reduces the laser scribing process to one step and lowers the requirements for the laser (expensive femtosecond or picosecond lasers are not required; ordinary nanosecond lasers are sufficient). Only a laser with edge-cleaning capabilities is needed to complete the process, and the simplified process significantly improves the product yield.

[0042] This invention can completely isolate the contact between the first conductive layer and the second conductive layer, as well as the contact between the first electrode and the electrochromic layer, greatly reducing the risk of short circuits and simplifying the process. In particular, after leaving the vacuum chamber, the electrochromic glass is extremely susceptible to water and oxygen erosion and damage. This solution can significantly reduce processing time and improve work efficiency.

[0043] The electrochromic glass provided by this invention has the characteristics of being suitable for large-area preparation, having good material stability, and having a long service life. It is expected to be used in active control energy-saving glass for building curtain walls and exterior windows, and has a broad market prospect.

[0044] The above description is merely an overview of the technical solution of the present invention. In order to better understand the technical means of the present invention and to implement it in accordance with the contents of the specification, the preferred embodiments of the present invention are described in detail below. Attached Figure Description

[0045] Figure 1 This is a schematic diagram of the structure of the electrochromic glass according to an embodiment of the present invention;

[0046] Figure 2 for Figure 1 A schematic diagram of the electrochromic layer;

[0047] Figure 3 This is a process flow diagram of the preparation method of electrochromic glass according to an embodiment of the present invention. Detailed Implementation

[0048] To further illustrate the technical means and effects adopted by the present invention to achieve the intended purpose, the following detailed description, in conjunction with preferred embodiments, provides a detailed explanation of the specific implementation methods, structures, features, and effects of an electrochromic glass, its preparation method, and its application according to the present invention. In the following description, different "embodiments" or "embodiments" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics in one or more embodiments can be combined in any suitable manner.

[0049] like Figure 1 As shown, the present invention provides an electrochromic glass, comprising a glass substrate 1, a first conductive layer 2 on the glass substrate 1, a laser groove 3 on the first conductive layer 2, a first electrode layer 6, an insulating layer 5 and an electrochromic layer 4 sequentially disposed on the first conductive layer 2, a second conductive layer 7 on the electrochromic layer 4, a protective layer 9 and a second electrode layer 8 sequentially disposed on the second conductive layer 7, and a protective layer 9 disposed on the second electrode layer 8.

[0050] In some embodiments of the present invention, a protective layer 9 is provided on both the first electrode layer 6 and the insulating layer 5. The protective layer 9 serves to protect the electrochromic layer 4, preventing scratches and moisture erosion on the one hand, and confining the current in the second conductive layer 7 on the other hand. In addition, the protective layer 9 helps to reduce defects in the laminated glass (delamination, bubbles, etc.) and also serves as an anti-reflective film to improve the glass transmittance.

[0051] In some embodiments of the present invention, the electrochromic layer 4 is located above the laser groove 3 to reduce short circuits caused by the connection between the first conductive layer 2 and the second electrode, increase the process window, and improve production efficiency.

[0052] In some embodiments of the present invention, the first conductive layer 2 or the second conductive layer 7 is selected from one of indium tin oxide, tin fluoride, and zinc oxide aluminum-doped graphene, preferably indium tin oxide, which has high conductivity, mature technology, and good weather resistance. The thickness of the first conductive layer 2 or the second conductive layer 7 is 200nm-350nm, preferably 300nm. If it is too thin, the resistance is high, the voltage applied to the electrochromic layer decreases, and the color change range is reduced; if it is too thick, the cost increases.

[0053] In other embodiments of the present invention, the number of lines in the laser groove 3 is 5-50, preferably 10-30. Too few lines will greatly increase the risk of short circuit between the upper and lower electrodes, while too many lines will reduce the discoloration area and easily cause local arcing during the coating process, resulting in glass defects. The width of the laser groove 3 is 0.02mm-0.2mm, preferably 0.05mm-0.1mm. Too narrow a width will easily cause inconsistent line depths and may cause bridging, failing to provide isolation. Too wide a width will increase processing time, reduce depth control accuracy, and easily cause excessively deep local areas. The depth of the laser groove 3 is 200nm-500nm, preferably 300-400nm. Too shallow a depth will not achieve the purpose of isolating the upper and lower conductive layers, while too deep a depth will easily cause local arcing during the coating process, resulting in glass defects. Furthermore, the coating layer will find it difficult to fill the groove, resulting in a large groove in the coating area, which is not conducive to close contact between the second electrode and the second conductive layer, and may even cause disconnection.

[0054] In other embodiments of the present invention, the width of the first electrode layer 6 or the second electrode layer 8 is 1mm-30mm, and the resistance is 5Ω / km-12Ω / km. The purpose of providing the first electrode layer 6 or the second electrode layer 8 is to facilitate connection to the positive or negative terminal of the power supply. The width is preferably 2mm-10mm, more preferably 5mm, and the preferred resistance is 8Ω / km. If the width of the first electrode layer 6 or the second electrode layer 8 (busbar) is too small, the DC resistance will be too large, reducing the effective voltage applied to the electrochromic glass, which is not conducive to the color change. If the width is too large, the DC resistance will be small, but on the one hand, it will greatly increase the cost, and on the other hand, it will reduce the color-changing area, affecting the aesthetics.

[0055] In other embodiments of the present invention, the first electrode layer 6 includes a plurality of first electrodes with a width of 0.02mm-2mm, preferably 0.05mm-1mm, and a thickness of 200nm-500nm, preferably 300nm-400nm. If the width is small and the thickness is thin, the resistance increases, the voltage effectively applied to the electrochromic layer decreases, which is not conducive to color change, and it is also inconvenient to connect wires, but it can increase the effective color-changing area of ​​the glass and improve the aesthetics. If the width is large and the thickness is thick, the resistance decreases, the voltage effectively applied to the electrochromic layer increases, which is conducive to color change and facilitates the connection of wires, but the effective color-changing area of ​​the glass decreases, which is not conducive to the aesthetics. In addition, the increased thickness requires a corresponding increase in the film thickness in the subsequent lamination process, which increases the production cost and may also cause glass defects (bubbles, cracks). The second electrode layer 8 includes multiple second electrodes with a width of 0.02mm-2mm, preferably 0.05mm-1mm, and a thickness of 200nm-500nm, preferably 300nm-400nm. Decreasing the thickness increases the resistance, which is detrimental to the application of the effective voltage; increasing the thickness decreases the resistance, which is beneficial to the application of the effective voltage, but reduces the transmittance, affecting the electrochromic effect. The material of the first or second electrode is selected from conductive silver paste, indium and its alloys, or tin and its alloys; preferably, it is conductive silver paste, which has a low processing temperature, high conductivity, and low contact resistance with the film layer.

[0056] In other embodiments of the present invention, the insulating layer 5 may be selected from thermosetting materials or UV-curable materials, and its width is 0.1 mm to 20 mm; preferably, the insulating layer 5 is selected from one of silicone, polyethylene, polyimide, polyphenylene sulfide, polyphenylene ether, polyarylate, polyetheretherketone, polyarylsulfone, and polyester resin; more preferably, the insulating layer 5 is silicone, polyimide, polyphenylene sulfide, or polyphenylene ether, and its outgassing rate is less than 5e-4 Pa, because these materials are resistant to high temperature, have low outgassing, and form fewer defects.

[0057] In some other embodiments of the present invention, the width of the insulating layer 5 is 0.1mm-20mm; preferably 2mm-3mm. This preferred width is small, which can increase the color-changing area and is beneficial to aesthetics. If the width is too small, it is not conducive to the isolation between the first electrode and the second conductive layer. If the width is too large, the effective color-changing area of ​​the glass will be reduced.

[0058] In other embodiments of the invention, such as Figure 2As shown, the electrochromic layer 4 includes a tungsten oxide film 41, a lithium oxide film 42, and a nickel-tungsten oxide film 43 sequentially deposited on the first conductive layer 2; the thickness of the tungsten oxide film 41 is 120nm-130nm; the thickness of the lithium oxide film 42 is 200nm-350nm; the thickness of the nickel-tungsten oxide film 43 is 65nm-80nm; and the total thickness of the electrochromic layer is 380nm-600nm.

[0059] In other embodiments of the present invention, the protective layer 9 is made of aluminum silicate, silicon oxide, niobium oxide, titanium oxide, or zirconium oxide, preferably aluminum silicate, with a thickness ranging from 170 nm to 220 nm. This design prevents scratches and moisture erosion, confines the current to the second conductive layer 2, and helps reduce defects in the laminated glass (delamination, bubbles, etc.). It also acts as an anti-reflective coating, improving glass transmittance. If the layer is too thin, it will not achieve the above effects; if it is too thick, the increased stress may cause delamination, and it will not provide anti-reflective protection, thus reducing glass transmittance.

[0060] like Figure 3 As shown, the present invention also provides a method for preparing electrochromic glass, comprising the following steps:

[0061] The first glass cleaning is performed to remove contaminants from both the top and bottom surfaces of the glass.

[0062] Deposit the first conductive layer;

[0063] Laser scribing of the first conductive layer;

[0064] An insulating layer is prepared on the first conductive layer;

[0065] Prepare the first electrode layer;

[0066] Depositing an electrochromic layer;

[0067] Deposit a second conductive layer;

[0068] A second electrode layer is fabricated on the second conductive layer;

[0069] Deposition protective layer.

[0070] In some other embodiments of the present invention, the preparation of the first conductive layer specifically includes the following steps: the preparation of the first conductive layer is completed by reactive magnetron sputtering, wherein the preparation of the first conductive layer specifically includes the following steps: vacuum reactive magnetron sputtering is used for coating, with an ITO target, argon gas at 350 sccm-400 sccm, vacuum degree at 0.3 Pa-0.6 Pa, coating temperature at 200℃-250℃, power at 9 kW, target burn-in for at least 5 min, oxygen flow at 7 sccm-9 sccm, and after the voltage and current stabilize, glass coating is started at a coating speed of 0.1 m / min-1 m / min, and the temperature is held at 200℃-250℃ for 20 min-60 min to complete the preparation of the first conductive layer, the thickness of which is 200 nm-350 nm.

[0071] In the above technical solution, laser scribing of the first conductive layer specifically includes the following steps: laser scribing is performed on the first conductive layer; specifically, an IGP green 30W laser with a power of 27W and a frequency of 50kHz is used to scribble 5-50 lines at the required positions on the first conductive layer, with each line spaced 0.02-0.2mm apart and a depth of 200nm-500nm. After scribing, the resistance inside and outside the scribing is tested to ensure that the resistance value is greater than 1 megohm; the purpose of laser scribing the first conductive layer 2 is to prevent short circuits between the upper and lower first and second conductive layers, disconnect the first conductive layer, and ensure that the resistance value is greater than 1 megohm.

[0072] Furthermore, the laser used in the first conductive layer 2 for laser scribing is an infrared laser, a green laser, an ultraviolet laser, or a picosecond laser; considering cost, an infrared laser is preferred, and a neodymium-doped yttrium aluminum garnet crystal infrared laser is more preferred, which reduces the requirement for laser scribing depth, increases the process window, improves production efficiency, and increases the yield.

[0073] In the above technical solution, the preparation of the insulating layer 5 on the first conductive layer 2 specifically includes the following steps: dispensing adhesive onto the first conductive layer and air-cooling to form the insulating layer; specifically, the insulating raw material is placed in the heating loading container of the dispensing machine, the insulating material is locally heated, and pressure is applied to the upper part of the container to generate downward pressure, which is then extruded from the dispensing needle in a linear shape and contacts the glass. The insulating layer is then formed by air cooling, with a width of 0.1mm-20mm. The purpose of preparing the insulating layer on the first conductive layer is to prevent short circuits between the first and second conductive layers, thus achieving physical isolation between them. A 1.8mm diameter needle is selected for the dispensing needle. The dispensing focus is coarsely adjusted, and then, on a sample glass plate of the same thickness, a "U" shape is applied. The line shape of the dispensing is observed, and the dispensing focus is finely adjusted in 0.01mm increments until the dispensing is linear, uniform, flat, and of uniform thickness. To ensure the stability of the insulating layer, it is generally applied twice. The diameter of the air bubbles between the glass insulating layer and the conductive layer is less than 0.2mm, and the number of air bubbles is less than 2 per meter. If air bubbles are present, the insulating layer will separate from the conductive layer, failing to provide insulation. This is especially true under vacuum conditions, where the bubbles enlarge, rendering the insulating layer ineffective. The air velocity for the air-cooling molding process is 10m / s-50m / s. If it is too low, the molding process will be slow, resulting in defects; if it is too high, the molding process will be fast, but the contact with the substrate will be weak.

[0074] In the technical solution of this invention, the preparation of an insulating layer on a first conductive layer specifically includes the following steps: placing an insulating material on the surface of the first conductive layer, then applying pressure to the insulating material on both sides of the first conductive layer, and using local heating to make it in close contact with the conductive layer; specifically, placing the insulating layer directly on the glass surface, applying pressure to the insulating material on both sides of the glass to make it in close contact with the glass, and then using local heating to make it in close contact with the conductive layer. Local heating can be achieved by using a fixed-point heater, such as a hair dryer, to heat the insulating layer.

[0075] If polyimide is chosen as the insulating raw material, the heating temperature should be set to 450℃-550℃, preferably 500℃. Too high a temperature will cause the silicone to decompose, while too low a temperature will prevent it from reaching a molten state. If silicone is chosen, the heating temperature should be set to 350℃-450℃, preferably 400℃. Too high a temperature will cause the silicone to decompose, while too low a temperature will prevent it from reaching a molten state. The pressure applied to the upper part of the container should be 100N-500N, preferably 300N. If the pressure is too low, the efficiency will be slow; if the pressure is too high, it will be difficult to control.

[0076] The order of preparing the insulating layer and the first electrode layer can be reversed. To improve production efficiency, they can be prepared together, for example, by using two dispensing machines to complete the dispensing separately. Preferably, the conductive layer is prepared first, which is beneficial for glass cleaning and reduces the formation of defects. While ensuring the cleanliness of the glass surface, they can be prepared simultaneously or in reverse order.

[0077] In addition, the preparation of the first electrode layer specifically includes the following steps: take 30ml-50ml of conductive silver paste and add it to the dispensing equipment, set the dispensing focus and dispensing position, run the equipment, the dispensing width is 0.02mm-2mm, and the thickness is 200nm-500nm. After the dispensing is completed, use a curing cabinet to heat and dry at 120℃-350℃ to complete the preparation of the first electrode layer; the first electrode layer includes multiple first electrodes, the width of which is 0.02mm-2mm and the thickness is 200nm-500nm.

[0078] The preparation of the electrochromic layer specifically includes the following steps: The electrochromic layer is prepared using reactive magnetron sputtering. First, a tungsten oxide thin film is prepared on the first conductive layer using a magnetron sputtering tungsten target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 40-50 sccm and the oxygen flow rate at 60-70 sccm, maintaining a working pressure of 0.6 Pa-0.65 Pa, and a film thickness of 120 nm-130 nm. Subsequently, a lithium oxide thin film is prepared on the tungsten oxide thin film using a magnetron sputtering lithium oxide target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled... The working pressure is maintained at 0.4 Pa to 0.45 Pa, and the film thickness is 200 nm to 350 nm. Then, a nickel-tungsten oxide film is prepared on a lithium oxide film using a magnetron sputtering nickel target. Argon gas is introduced into the vacuum chamber, and the flow rate of argon gas is controlled at 40 sccm to 50 sccm, and the flow rate of oxygen is controlled at 100 sccm to 120 sccm. The working pressure is maintained at 0.6 Pa to 0.7 Pa, and the film thickness is 65 nm to 80 nm. The total thickness of the electrochromic layer is 380 nm to 600 nm.

[0079] In implementing this invention, the preparation of the second conductive layer specifically includes the following steps:

[0080] Vacuum reactive magnetron sputtering was used for coating with an ITO target, argon gas at 400-500 sccm, vacuum at 0.4-0.55 Pa, coating temperature at 200-250℃, power at 9-10 kW for at least 5 minutes to burn the target, oxygen was introduced at 7-9 sccm, and once the voltage fluctuated within 370-390V, glass coating began at a coating speed of 0.5-1 m / min, and held at 200-250℃ for 20-60 minutes to complete the preparation of the second conductive layer with a thickness of 200-350 nm.

[0081] In some embodiments of the present invention, the preparation of the second electrode layer on the second conductive layer specifically includes the following steps: taking 30ml-50ml of silver paste and adding it to the dispensing equipment, setting the dispensing focus and dispensing position, running the equipment, the dispensing width is 0.02mm-2mm and the thickness is 200nm-500nm, after the dispensing is completed, using a curing cabinet to heat and dry at 120℃-350℃ to complete the preparation of the second electrode.

[0082] In some embodiments of the present invention, the deposition of the protective layer specifically includes the following steps: vacuum reactive magnetron sputtering deposition is performed using a silicon target, argon gas at 600 sccm-700 sccm is introduced, and a power of 9 KW-11 KW is used to first burn the target, then oxygen at 300 sccm-350 sccm is introduced, and after the current and voltage stabilize, the deposition begins to complete the preparation of the protective layer, which has a thickness of 170 nm-220 nm.

[0083] The present invention also provides a building curtain wall, the building curtain wall comprising the above-mentioned electrochromic glass.

[0084] The present invention also provides an exterior window, the exterior window comprising actively adjustable energy-saving glass, the actively adjustable energy-saving glass comprising the above-mentioned electrochromic glass.

[0085] The present invention will be further described below with reference to specific embodiments, but this should not be construed as a limitation on 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 description of the present invention still fall within the scope of protection of the present invention.

[0086] In the following embodiments of the present invention, unless otherwise specified, all components involved are commercially available products well known to those skilled in the art, and unless otherwise specified, all methods involved are conventional methods.

[0087] Example 1

[0088] First, ordinary 2mm thick ultra-clear glass is cleaned. After cleaning, vacuum reactive magnetron sputtering is used for coating. ITO target, argon gas is 400 sccm, vacuum degree is 0.4pa, coating temperature is 200℃, power is 9KW, target burn-in is 5min, oxygen is purged at 9 sccm, and when the voltage reaches 370V, glass coating begins. The coating speed is 0.5m / min, the coating thickness is 300nm, and the temperature is held at 200℃ for 60min to complete the preparation of the first conductive layer.

[0089] Laser scribing is performed on the first conductive layer using a power of 27W and a frequency of 50kHz, scribing a laser groove 30mm inward from the glass edge. The number of laser grooves is 10; the width of the laser groove is 0.1mm; and the depth of the laser groove is 350nm. After scribing, a conventional electrostatic blowing device is used to clean the surface of the first conductive layer.

[0090] Then, an insulating material (polyimide) with a width of 0.5 mm is placed on the first conductive layer. After that, a pressure of 300 N is applied to the insulating material on both sides of the first conductive layer using a pressure strip. The insulating material is heated to 500 °C by a heat lamp strip to make it come into close contact with the conductive layer, thus obtaining the insulating layer.

[0091] Then, the first electrode layer is prepared on the first conductive layer by applying conductive silver paste. 30 ml of conductive silver paste is added to the dispensing equipment, the dispensing focus and position are set, the equipment is run, the dispensing width is 1 mm and the thickness is 400 nm. After dispensing, the first electrode layer is dried at 120 °C in a curing cabinet to complete the preparation of the first electrode layer. The first electrode layer includes a first electrode with a width of 1 mm and a thickness of 400 nm.

[0092] Next, an electrochromic layer is prepared on the first conductive layer. First, a tungsten oxide film is prepared on the first conductive layer using a magnetron sputtering tungsten target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 50 sccm and the oxygen flow rate at 70 sccm, maintaining a working pressure of 0.6 Pa. The sputtering time is controlled to achieve a tungsten oxide film thickness of 120 nm. Then, a lithium oxide film is prepared on the tungsten oxide film using a magnetron sputtering lithium oxide target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 20 sccm, maintaining a working pressure of 0.4 Pa. The sputtering time is controlled to achieve a lithium oxide film thickness of 200 nm. Then, a nickel-tungsten oxide film is prepared on the lithium oxide film using a magnetron sputtering nickel target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 50 sccm and the oxygen flow rate at 100 sccm, maintaining a working pressure of 0.6 Pa. The sputtering time is controlled to achieve a nickel-tungsten oxide film thickness of 65 nm. The total thickness of the electrochromic layer is 385 nm.

[0093] After the electrochromic layer is prepared, the second conductive layer is prepared on it. Vacuum reactive magnetron sputtering is used for coating, with an ITO target, an argon flow rate of 400 sccm, a vacuum degree of 0.4 Pa, a coating temperature of 200℃, a power of 9KW, a target burn-in time of 5 min, oxygen flow of 9 sccm, and coating starting when the voltage reaches 370V. The coating speed is 0.5 m / min, the coating thickness is 300 nm, and the temperature is held at 200℃ for 60 min to complete the preparation of the second conductive layer.

[0094] Then, a second electrode layer was prepared on the second conductive layer by applying conductive silver paste. 30 ml of conductive silver paste was added to the dispensing equipment, the dispensing focus and position were set, the equipment was run, the dispensing width was 1 mm and the thickness was 400 nm. After dispensing, the second electrode layer was dried at 120 °C in a curing cabinet to complete the preparation of the second electrode layer. The second electrode layer includes a second electrode with a width of 1 mm and a thickness of 400 nm.

[0095] Finally, vacuum reactive magnetron sputtering was used to deposit silicon oxide. Argon gas was introduced into the vacuum chamber at a flow rate of 600 sccm and a power of 9 kW. The target was first burned, and then oxygen was introduced at a flow rate of 300 sccm while maintaining a working pressure of 0.56 Pa. The film thickness was 190 nm, thus completing the preparation of the protective layer.

[0096] Example 2

[0097] First, a 2mm thick ordinary ultra-clear glass was taken out and cleaned. After cleaning, vacuum reactive magnetron sputtering was used for coating. The ITO target was used, the argon gas was 400 sccm, the vacuum degree was 0.4pa, the coating temperature was 200℃, the power was 9KW, the target was burned for 5min, oxygen was introduced at 9 sccm, and when the voltage reached 370V, the glass coating was started. The coating speed was 0.5m / min, the coating thickness was 300nm, and the temperature was held at 200℃ for 60min to complete the preparation of the first conductive layer.

[0098] Laser scribing is performed on the first conductive layer using a power of 27W and a frequency of 50kHz, scribing a laser groove 30mm inward from the glass edge. The number of laser grooves is 10; the width of the laser groove is 0.1mm; and the depth of the laser groove is 350nm. After scribing, a conventional electrostatic blowing device is used to clean the surface of the first conductive layer.

[0099] Then, an insulating material (polyimide) with a width of 2 mm is placed on the first conductive layer. After that, a pressure of 300 N is applied to the insulating material on both sides of the first conductive layer using a pressure strip. The insulating material is heated to 500 °C by a heat lamp strip to make it come into close contact with the conductive layer, thus obtaining the insulating layer.

[0100] Then, the first electrode layer is prepared on the first conductive layer by applying conductive silver paste. 30 ml of conductive silver paste is added to the dispensing equipment, the dispensing focus and position are set, the equipment is run, the dispensing width is 1 mm and the thickness is 400 nm. After dispensing, the first electrode layer is dried at 120 °C in a curing cabinet to complete the preparation of the first electrode layer. The first electrode layer includes a first electrode with a width of 1 mm and a thickness of 400 nm.

[0101] Next, an electrochromic layer is prepared on the first conductive layer. First, a tungsten oxide thin film is prepared on the first conductive layer using a magnetron sputtering tungsten target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 50 sccm and the oxygen flow rate at 70 sccm, maintaining a working pressure of 0.6 Pa. The sputtering time is controlled to achieve a tungsten oxide film thickness of 120 nm. Then, a lithium oxide thin film is prepared on the tungsten oxide film. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 20 sccm, maintaining a working pressure of 0.4 Pa. The sputtering time is controlled to achieve a lithium oxide film thickness of 200 nm. Then, a nickel-tungsten oxide thin film is prepared using a magnetron sputtering nickel target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 50 sccm and the oxygen flow rate at 100 sccm, maintaining a working pressure of 0.6 Pa. The sputtering time is controlled to achieve a nickel-tungsten oxide thin film thickness of 65 nm. The total thickness of the electrochromic layer is 385 nm.

[0102] After the electrochromic layer is prepared, the second conductive layer is prepared on it. Vacuum reactive magnetron sputtering is used for coating, with an ITO target, an argon flow rate of 400 sccm, a vacuum degree of 0.4 Pa, a coating temperature of 200℃, a power of 9KW, a target burn-in time of 5 min, oxygen flow of 9 sccm, and when the voltage reaches 370V, glass coating begins at a coating speed of 0.5 m / min and a coating thickness of 300 nm. The coating is held at 200℃ for 60 min to complete the preparation of the second conductive layer.

[0103] Then, a second electrode layer was prepared on the second conductive layer by applying conductive silver paste. 30 ml of conductive silver paste was added to the dispensing equipment, the dispensing focus and position were set, the equipment was run, the dispensing width was 1 mm and the thickness was 400 nm. After dispensing, the second electrode layer was dried at 120 °C in a curing cabinet to complete the preparation of the second electrode layer. The second electrode layer includes a second electrode with a width of 1 mm and a thickness of 400 nm.

[0104] Finally, vacuum reactive magnetron sputtering was used for coating silicon oxide. First, a silicon oxide thin film was prepared using a magnetron sputtering silicon target. Argon gas was introduced into the vacuum chamber, and the flow rate of argon gas was controlled at 600 sccm. Using a power of 9 kW, the target was first burned, and then oxygen gas was introduced at 300 sccm. The working pressure was maintained at 0.56 Pa, and the film thickness was 190 nm, thus completing the preparation of the protective layer.

[0105] Example 3

[0106] First, take out ordinary 2mm thick ultra-clear glass and clean it. After cleaning, vacuum reactive magnetron sputtering is used for coating. ITO target, argon gas 400sccm, vacuum degree 0.4pa, coating temperature 200℃, power 9KW, target burn-in 5min, oxygen 9sccm, when the voltage reaches 370V, glass coating begins, coating speed is 0.5m / min, coating thickness is 300nm, hold at 200℃ for 60min to complete the preparation of the first conductive layer.

[0107] Laser scribing is performed on the first conductive layer using a power of 27W and a frequency of 50kHz, scribing a laser groove 30mm inward from the glass edge. The number of laser grooves is 10; the width of the laser groove is 0.1mm; and the depth of the laser groove is 350nm. After scribing, a conventional electrostatic blowing device is used to clean the surface of the first conductive layer.

[0108] Then, polyimide insulating material with a width of 5mm is placed on the first conductive layer. After that, 300N pressure is applied to the insulating material on both sides of the first conductive layer using a pressure strip. The insulating material is heated to 500℃ by the heat lamp strip to make it come into close contact with the conductive layer, thus obtaining the insulating layer.

[0109] Then, the first electrode is prepared on the first conductive layer by applying conductive silver paste. 30 ml of conductive silver paste is added to the dispensing equipment, the dispensing focus and position are set, the equipment is run, the dispensing width is 1 mm and the thickness is 400 nm. After dispensing, the first electrode is dried at 120 °C in a curing cabinet to complete the preparation of the first electrode. The first electrode layer includes the first electrode, which has a width of 1 mm and a thickness of 400 nm.

[0110] Next, an electrochromic layer is prepared on the first conductive layer. First, a tungsten oxide thin film is prepared on the first conductive layer using a magnetron sputtering tungsten target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 50 sccm and the oxygen flow rate at 70 sccm, maintaining a working pressure of 0.6 Pa. The sputtering time is controlled to achieve a tungsten oxide film thickness of 120 nm. Then, a lithium oxide thin film is prepared on the tungsten oxide film. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 20 sccm, maintaining a working pressure of 0.4 Pa. Sputtering deposition is performed on the tungsten oxide surface, with the sputtering time controlled to achieve a lithium oxide film thickness of 200 nm. Then, a nickel-tungsten oxide thin film with a nickel storage layer is prepared using a magnetron sputtering nickel target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 50 sccm and the oxygen flow rate at 100 sccm, maintaining a working pressure of 0.6 Pa. The sputtering time is controlled to achieve a nickel-tungsten oxide thin film thickness of 65 nm. The total thickness of the electrochromic layer is 385 nm.

[0111] After the electrochromic layer is prepared, the second conductive layer is prepared on it. Vacuum reactive magnetron sputtering is used for coating, with an ITO target, an argon flow rate of 400 sccm, a vacuum degree of 0.4 Pa, a coating temperature of 200℃, a power of 9KW, a target burn-in time of 5 min, oxygen flow of 9 sccm, and when the voltage reaches 370V, glass coating begins at a coating speed of 0.5 m / min, with a required coating thickness of 300 nm. The coating is held at 200℃ for 60 min to complete the preparation of the second conductive layer.

[0112] Then, a second electrode layer was prepared on the second conductive layer by applying conductive silver paste. 30 ml of conductive silver paste was added to the dispensing equipment, the dispensing focus and position were set, the equipment was run, the dispensing width was 1 mm and the thickness was 400 nm. After dispensing, the second electrode layer was dried at 120 °C in a curing cabinet to complete the preparation of the second electrode layer. The second electrode layer includes a second electrode with a width of 1 mm and a thickness of 400 nm.

[0113] Finally, vacuum reactive magnetron sputtering was used for coating silicon oxide. First, a silicon oxide thin film was prepared using a magnetron sputtering silicon target. Argon gas was introduced into the vacuum chamber, and the flow rate of argon gas was controlled at 600 sccm. Using a power of 9 kW, the target was first burned, and then oxygen gas was introduced at 300 sccm. The working pressure was maintained at 0.56 Pa, and the film thickness was 190 nm, thus completing the preparation of the protective layer.

[0114] Comparative Example 1

[0115] First, ordinary 2mm thick ultra-clear glass is cleaned. After cleaning, vacuum reactive magnetron sputtering is used for coating. ITO target, argon gas is 400 sccm, vacuum degree is 0.4pa, coating temperature is 200℃, power is 9KW, target burn-in is 5min, oxygen is purged at 9 sccm, and when the voltage reaches 370V, glass coating begins. The coating speed is 0.5m / min, the coating thickness is 300nm, and the temperature is held at 200℃ for 60min to complete the preparation of the first conductive layer.

[0116] Laser scribing is performed on the first conductive layer using a power of 27W and a frequency of 50kHz, scribing a laser groove 30mm inward from the glass edge. The number of laser grooves is 10; the width of the laser groove is 0.1mm; and the depth of the laser groove is 350nm. After scribing, a conventional electrostatic blowing device is used to clean the surface of the first conductive layer.

[0117] Then, an electrochromic layer is prepared on the first conductive layer. First, a tungsten oxide film is prepared on the first conductive layer using a magnetron sputtering tungsten target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 50 sccm and the oxygen flow rate at 70 sccm, maintaining a working pressure of 0.6 Pa. The thickness of the tungsten oxide film is 120 nm by controlling the sputtering time. Subsequently, a lithium oxide film is prepared on the tungsten oxide film using a magnetron sputtering lithium oxide target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 20 sccm, maintaining a working pressure of 0.4 Pa. The thickness of the lithium oxide film is 200 nm by controlling the sputtering time. Then, a nickel-tungsten oxide film is prepared on the lithium oxide film using a magnetron sputtering nickel target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 50 sccm and the oxygen flow rate at 100 sccm, maintaining a working pressure of 0.6 Pa. The thickness of the nickel-tungsten oxide film is 65 nm by controlling the sputtering time. The total thickness of the electrochromic layer is 385 nm.

[0118] After the electrochromic layer was prepared, the second conductive layer was prepared on it. Vacuum reactive magnetron sputtering was used for coating, with an ITO target, an argon flow rate of 400 sccm, a vacuum degree of 0.4 Pa, a coating temperature of 200℃, a power of 9 kW, a target burn-in time of 5 min, oxygen flow of 9 sccm, and coating started when the voltage reached 370 V. The coating speed was 0.5 m / min, the coating thickness was 300 nm, and the temperature was maintained at 200℃ for 60 min to complete the preparation of the second conductive layer.

[0119] Next, laser scribing is performed on the second conductive layer using 27W power and 100kHz frequency, 30mm inward from the glass edge, to create 10 laser grooves; the width of each groove is 0.1mm and the depth is 650nm, to isolate the second conductive layer. Then, laser scribing is performed on the second conductive layer again using 27W power and 150kHz frequency, 20mm inward from the glass edge, to create 10 laser grooves; the width of each groove is 0.1mm and the depth is 1000nm. After scribing, a conventional electrostatic blowing device is used to clean the surface of the second conductive layer.

[0120] Then, the first electrode layer is prepared by dispensing conductive silver paste. 30 ml of silver paste is added to the dispensing equipment, the dispensing focus and dispensing position are set, the equipment is run, the dispensing width is 1 mm and the thickness is 400 nm. After dispensing, the silver paste is baked by heating at 120 °C in a curing cabinet to complete the preparation of the first electrode layer. The first electrode layer includes a first electrode with a width of 1 mm and a thickness of 400 nm.

[0121] Then, the second electrode layer is prepared by dispensing conductive silver paste. 30 ml of silver paste is added to the dispensing equipment, the dispensing focus and position are set, the equipment is run, the dispensing width is 1 mm and the thickness is 400 nm. After dispensing, the silver paste is baked by heating at 120 °C in a curing cabinet to complete the preparation of the second electrode layer. The second electrode layer includes a second electrode with a width of 1 mm and a thickness of 400 nm.

[0122] Finally, vacuum reactive magnetron sputtering was used to deposit silicon oxide. Argon gas was introduced into the vacuum chamber at a flow rate of 600 sccm and a power of 9 kW. The target was burned first, and then oxygen was introduced at a flow rate of 300 sccm. The working pressure was maintained at 0.56 Pa, and the film thickness was 190 nm, thus completing the preparation of the protective layer.

[0123] The main preparation process of Examples 1-3 and Comparative Example 1 and the properties of the obtained electrochromic glass are shown in Tables 1 and 2.

[0124] Table 1. Main preparation process flow of Examples 1-3 and Comparative Example 1

[0125]

[0126] Table 2 Performance tests of the electrochromic glasses obtained in Examples 1-3 and Comparative Example 1

[0127] Example 1 Example 2 Example 3 Comparative Example 1 Product yield (%) 65％ 70％ 70％ 60％ Product appearance Good Good Fair Good Device current 53 mA 22 mA 21 mA 200 mA Cycle life 67,300 times 70,500 times 71,350 times 50,000 times

[0128] As can be seen from the data in Tables 1 and 2, compared with the electrochromic glass of Comparative Example 1, the manufacturing process of the electrochromic glass in Examples 1-3 is reduced, and the addition of an insulating layer (isolation material) more effectively isolates the upper and lower conductive layers, preventing electrode short circuits. The electrochromic glass of Examples 1-3 has a significantly lower current than that of Comparative Example 1, resulting in greater energy savings and more stable performance. The cycle life of the electrochromic glass of Examples 1-3 is increased by more than 35% compared with that of Comparative Example 1 (for example, reaching more than 40%, such as 41% or 43%), and the product qualification rate is greatly improved.

[0129] In the above embodiments, the descriptions of each embodiment have different focuses. For parts not described in detail in a certain embodiment, please refer to the relevant descriptions in other embodiments.

[0130] The numerical range described in this invention includes all values ​​within this range, and also includes any range value composed of any two values ​​within this range. Different values ​​of the same indicator appearing in all embodiments of this invention can be arbitrarily combined to form a range value.

[0131] The technical features in the claims and / or specification of this invention can be combined, and the combination is not limited to the combinations obtained through reference in the claims. Technical solutions obtained by combining the technical features in the claims and / or specification are also within the scope of protection of this invention.

[0132] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Any simple modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention shall still fall within the scope of the technical solution of the present invention.

Claims

1. A method for preparing electrochromic glass, characterized in that, The preparation method includes the following steps: First glass cleaning; Deposit the first conductive layer; Laser scribing of the first conductive layer; An insulating layer is prepared on the first conductive layer; Prepare the first electrode; Depositing an electrochromic layer; Deposit a second conductive layer; A second electrode is fabricated on the second conductive layer; Deposition protective layer; The preparation of the insulating layer on the first conductive layer specifically includes the following steps: dispensing the insulating material onto the first conductive layer and air-cooling to form the insulating layer; the preparation of the first electrode layer specifically includes the following steps: adding 30ml-50ml of conductive silver paste to the dispensing equipment, setting the dispensing focus and position, the dispensing width being 0.02-2mm and the thickness being 200-500nm, and after dispensing, using a curing cabinet to heat and dry at 120℃-350℃ to complete the preparation of the first electrode layer; The electrochromic glass includes a glass substrate, a first conductive layer on the glass substrate, a laser groove on the first conductive layer, a first electrode layer, an insulating layer and an electrochromic layer sequentially disposed on the first conductive layer, a second conductive layer on the electrochromic layer, a protective layer and a second electrode layer on the second conductive layer, and a protective layer on the second electrode layer; the insulating layer is selected from thermosetting materials or UV-curable materials, and its width is 0.1mm-20mm.

2. The method for preparing electrochromic glass as described in claim 1, characterized in that, The first electrode layer and the insulating layer are both provided with protective layers; the electrochromic layer is located above the laser groove; the first conductive layer or the second conductive layer is selected from one of indium tin oxide layer, tin fluoride oxyfluoride layer and aluminum-doped zinc oxide graphene layer, and its thickness is 200nm-350nm.

3. The method for preparing electrochromic glass as described in claim 1, characterized in that, The laser groove has 5-50 lines; the width of the laser groove is 0.02-0.2 mm; the depth of the laser groove is 200-500 nm; the width of the first electrode layer or the second electrode layer is 1 mm-30 mm, and the resistance is 5-12 Ω / km; the first electrode layer includes multiple first electrodes with a width of 0.02-2 mm and a thickness of 200-500 nm; the second electrode layer includes multiple second electrodes with a width of 0.02-2 mm and a thickness of 200-500 nm; the material of the first electrode or the second electrode is selected from conductive silver paste, indium and its alloys, or tin and its alloys.

4. The method for preparing electrochromic glass as described in claim 1, characterized in that, The electrochromic layer comprises a tungsten oxide film, a lithium oxide film, and a nickel-tungsten oxide film sequentially deposited on a first conductive layer; the thickness of the tungsten oxide film is 120nm-130nm; the thickness of the lithium oxide film is 200nm-350nm; the thickness of the nickel-tungsten oxide film is 65nm-80nm; and the protective layer is aluminum silicate, silicon oxide, niobium oxide, titanium oxide, or zirconium oxide, with a thickness of 170-220nm.

5. The method for preparing electrochromic glass as described in claim 1, characterized in that, The preparation of the first conductive layer specifically includes the following steps: vacuum reactive magnetron sputtering deposition is performed using an ITO target, with argon gas at 400 sccm, a vacuum degree of 0.3 Pa-0.6 Pa, a deposition temperature of 200℃-250℃, a power of 9 kW for at least 5 minutes of target burning, oxygen flow of 7 sccm-9 sccm, and after the voltage and current stabilize, glass deposition begins at a deposition speed of 0.1 m / min-1 m / min, requiring a deposition thickness of 200 nm-350 nm, and holding at 200℃-250℃ for 20 minutes-60 minutes to complete the preparation of the first conductive layer; The laser scribing of the first conductive layer specifically includes the following steps: laser scribing on the first conductive layer; the laser used for laser scribing the first conductive layer is an infrared laser, a green laser, an ultraviolet laser, or a picosecond laser.

6. The method for preparing electrochromic glass as described in claim 1, characterized in that, The preparation of the electrochromic layer specifically includes the following steps: The electrochromic layer is prepared using reactive magnetron sputtering. First, a tungsten oxide thin film is prepared on the first conductive layer using a magnetron sputtering tungsten target. Argon gas is introduced into the vacuum chamber, with the argon flow rate controlled at 40-50 sccm and the oxygen flow rate at 60-70 sccm, maintaining a working pressure of 0.6 Pa-0.65 Pa. The thickness of the tungsten oxide thin film is 120 nm-130 nm. Subsequently, a lithium oxide thin film is prepared on the surface of the tungsten oxide thin film using a magnetron sputtering lithium oxide target. Argon gas is then introduced into the vacuum chamber. The process involves controlling the flow rate of argon gas at 15-20 sccm, maintaining the working pressure at 0.4 Pa-0.45 Pa, and forming a lithium oxide film with a thickness of 200 nm-350 nm. Then, a nickel-tungsten oxide film is prepared on the surface of the lithium oxide film using a magnetron sputtering nickel target. Argon gas is introduced into the vacuum chamber, with the flow rate controlled at 40-50 sccm and the oxygen flow rate at 100-120 sccm, maintaining the working pressure at 0.6 Pa-0.7 Pa, and forming a nickel-tungsten oxide film with a thickness of 65 nm-80 nm.

7. The method for preparing electrochromic glass as described in claim 1, characterized in that, The preparation of the second conductive layer specifically includes the following steps: Vacuum reactive magnetron sputtering is used for coating with an ITO target, argon gas at 400 sccm, vacuum at 0.3 Pa-0.6 Pa, coating temperature at 200℃-250℃, target burn-in at 9 kW for at least 5 minutes, oxygen flow at 7-9 sccm, and after the voltage and current stabilize, glass coating begins at a speed of 0.1 m / min-1 m / min, requiring a coating thickness of 200 nm-350 nm. The coating is held at 200℃-250℃ for 20-60 minutes to complete the preparation of the first conductive layer. The preparation of the second electrode layer on the second conductive layer specifically includes the following steps: 30 ml-50 ml of conductive silver paste is added to a dispensing device, the dispensing focus and position are set, the dispensing width is 0.02 mm-2 mm, and the thickness is 200 nm-500 nm. After dispensing, the paste is dried in a curing cabinet at 120℃-350℃ to complete the preparation of the second electrode layer. The specific steps for depositing the protective layer are as follows: vacuum reactive magnetron sputtering is used for film deposition. A silicon target is used, and argon gas at 600 sccm-700 sccm is introduced. A power of 9 KW-11 KW is used to first burn the target, and then oxygen at 300 sccm-350 sccm is introduced. After the current and voltage stabilize, film deposition begins. The silicon oxide thickness is 170 nm-220 nm, thus completing the preparation of the protective layer.

8. A building curtain wall, characterized in that, The building curtain wall comprises electrochromic glass prepared by the method of any one of claims 1-7.

9. An exterior window, characterized in that, The exterior window includes actively adjustable energy-saving glass, which includes electrochromic glass prepared by the method described in any one of claims 1-7.

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