Electrochromic film product as well as preparation method and application thereof

Abstract

The invention provides an electrochromic film product as well as a preparation method and application thereof. The electrochromic film product comprises a glass substrate and an electrochromic film layer, the preparation method comprises the following steps: in a vacuum cavity, carrying out vacuum plating on a glass substrate with an electrochromic film layer, and then carrying out vacuum baking treatment at the temperature of 200-400 DEG C for 30-120 minutes to obtain the electrochromic film product. Vacuum baking treatment is directly carried out in the vacuum cavity, no extra atmospheric baking equipment needs to be purchased, and the preparation cost of an electrochromic film product is reduced. And moreover, the product subjected to vacuum coating cannot be in contact with water vapor in the air, so that the pollution of the water vapor to the electrochromic film layer is avoided, and meanwhile, the problem of poor appearance of the product caused by dust in the air in the product carrying process is avoided.

Description

Technical Field

[0001] The present invention relates to the technical field of electrochromic materials, and in particular to an electrochromic thin film product and a preparation method and application thereof. Background Art

[0002] As the performance requirements of electrochromic products become higher and higher, there are certain requirements for the transmittance of fading and colored states, so the products will be heated after coating to improve the modulation amplitude performance of the products.

[0003] At present, the industry mainly uses additional atmospheric baking equipment, and after the vacuum coating is completed, it is moved to the atmospheric baking equipment for the film baking process.

[0004] In the existing atmospheric baking method, the film layer easily absorbs water vapor in the air during the process from the vacuum chamber to the atmospheric baking equipment, resulting in a decrease in film performance. At the same time, the atmospheric baking equipment is not as clean as the vacuum environment, which can easily lead to poor product appearance. In addition to the vacuum coating equipment, an additional set of atmospheric baking equipment needs to be purchased, which increases production costs.

[0005] CN111474792A discloses a porous electrochromic film and a preparation method, a multicolor electrochromic film and a preparation method, and an electrochromic device and a preparation method, comprising the following steps: providing a mixed solution of electrochromic materials; depositing the mixed solution of electrochromic materials on the surface of a substrate by electrostatic spraying to obtain a porous electrochromic film. The prepared porous electrochromic film has a porous structure, which is conducive to ion diffusion, can greatly improve the response speed of the electrochromic film, reduce the working voltage, has good stability, and has a simple preparation process. The conductive substrate can be replaced at will according to actual needs and material properties. It is suitable for large-area preparation of electrochromic films and related devices, including smart color-changing glass, display devices, and flexible or arbitrary curved devices.

[0006] CN115327827A discloses a method for preparing an electrochromic film component with a texture pattern, comprising: firstly plating a first transparent conductive layer on a first substrate plate, and then using a first laser to perform engraving; then plating an anode electrochromic layer, an ion conduction layer, a cathode electrochromic layer and a second transparent conductive layer in sequence, and then using a second laser to engrave away the stacked 5 film layers to form a graphic area and a blank area; then, using a third laser to engrave away the stacked 4 film layers except the first transparent conductive layer; then, respectively interconnecting the graphic area and the blank area with wires, and laminating with the second substrate; after lamination, performing protective packaging with the third substrate to obtain an electrochromic film component with a texture pattern; the preparation method uses laser technology to engrave the required pattern on the plated electrochromic functional layer, and realizes the mode conversion through the change of voltage, so that the electrochromic film component is more practical and beautiful.

[0007] CN115390328A discloses a flexible electrochromic electronic thin film component and a preparation method thereof, wherein the flexible electrochromic electronic thin film component comprises a separation layer, an adhesive layer, a flexible substrate layer, an electrochromic functional layer and a flexible protective layer which are sequentially stacked; the preparation method comprises adopting a magnetron sputtering method to plate the electrochromic functional layer on one side of the flexible substrate layer, and then pressing the electrochromic functional layer together with the flexible protective layer; and then sequentially installing an adhesive layer and a separation layer on the other side of the flexible substrate layer to obtain a flexible electrochromic electronic thin film component; the preparation method has a simple process flow, and the obtained product can be directly attached to existing equipment without disassembly and replacement to achieve an electrochromic effect, and has good economy.

[0008] However, none of the above-mentioned methods for preparing the electrochromic film solves the problem that the atmospheric baking process requires additional atmospheric baking equipment, which increases production costs. Summary of the invention

[0009] In view of the problems existing in the prior art, the present invention provides an electrochromic film product and a preparation method and application thereof, which directly performs vacuum baking in a vacuum chamber without the need to purchase additional atmospheric baking equipment, thereby reducing the preparation cost of the electrochromic film. Moreover, the vacuum-plated product will not come into contact with water vapor in the air, thus avoiding the contamination of the electrochromic film layer by water vapor, and at the same time avoiding the problem of poor appearance of the product caused by dust in the air during the transportation of the product.

[0010] To achieve this object, the present invention adopts the following technical solutions:

[0011] In a first aspect, the present invention provides a method for preparing an electrochromic thin film product, the preparation method comprising the following steps:

[0012] In a vacuum chamber, after vacuum plating an electrochromic thin film layer on a glass substrate, vacuum baking is performed at a temperature of 200 to 400° C. for 30 to 120 minutes to obtain the electrochromic thin film product;

[0013] The electrochromic thin film layer comprises a first transparent conductive layer, a cathode electrochromic layer, a lithium dielectric layer, an ion conduction layer, an anode electrochromic layer and a second transparent conductive layer which are sequentially arranged from a glass substrate outward.

[0014] The preparation method of the electrochromic thin film product described in the present invention directly performs vacuum baking treatment after completing vacuum coating in a vacuum chamber. The product does not need to leave the vacuum coating equipment, thus avoiding contact between the product and external water vapor. At the same time, there is less dust in the vacuum chamber, which effectively improves the appearance quality of the product. At the same time, the inherent vacuum coating equipment can complete both the coating and film post-baking processes, and there is no need to purchase additional atmospheric baking equipment separately, so that the same electrochromic thin film product as the prior art is obtained, achieving multiple goals at one stroke.

[0015] The temperature of the vacuum baking in the present invention is 200-400° C. When the temperature of the vacuum baking is too low or too high, the obtained electrochromic film may be partially ineffective, thus affecting subsequent normal use.

[0016] The temperature of the vacuum baking in the present invention is 200-400°C, for example, it can be 200°C, 220°C, 250°C, 300°C, 350°C, 380°C or 400°C, but it is not limited to the listed values, and other values ​​not listed in the numerical range are also applicable;

[0017] The time is 30 to 120 minutes, for example, it can be 30 minutes, 40 minutes, 50 minutes, 80 minutes, 90 minutes, 100 minutes or 120 minutes, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0018] In addition to the electrochromic film layer, other film layers can be added to the film layer vacuum-coated on the substrate according to the preparation method of the present invention according to actual conditions, so that the electrochromic thin film product has the required characteristics.

[0019] Preferably, the first transparent conductive layer comprises ITO conductive glass.

[0020] Preferably, the thickness of the first transparent conductive layer is 300-800 nm, for example, 300 nm, 350 nm, 400 nm, 500 nm, 600 nm, 700 nm or 800 nm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0021] Preferably, the first transparent conductive layer is coated by a magnetron sputtering process, and the process parameters include: power 2 to 10 kW, for example, 2 kW, 3 kW, 5 kW, 6 kW, 7 kW, 8 kW or 10 kW, etc., but are not limited to the listed values, and other values ​​not listed within the range are also applicable;

[0022] The coating temperature is 230-350°C, for example, it can be 230°C, 240°C, 250°C, 280°C, 300°C, 330°C or 350°C, but it is not limited to the listed values, and other values ​​not listed in the range are also applicable;

[0023] The coating pressure is 0.1-1.0 Pa, for example, it can be 0.1 Pa, 0.3 Pa, 0.5 Pa, 0.8 Pa, 0.9 Pa, 0.95 Pa or 1.0 Pa, etc., but it is not limited to the listed values, and other values ​​not listed in the range are also applicable;

[0024] The argon gas flow rate is 100 to 500 sccm, for example, 100 sccm, 150 sccm, 200 sccm, 300 sccm, 400 sccm, 450 sccm or 500 sccm, etc., but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable;

[0025] Oxygen concentration 0.1% to 1%, for example, can be 0.1%, 0.2%, 0.3%, 0.5%, 0.7%, 0.9% or 1%, etc., but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable;

[0026] The coating speed is 0.1 to 1.0 m / min, for example, it can be 0.1 m / min, 0.3 m / min, 0.4 m / min, 0.5 m / min, 0.7 m / min, 0.9 m / min or 1.0 m / min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0027] Preferably, the cathode electrochromic layer comprises WO x .

[0028] Preferably, the thickness of the cathode electrochromic layer is 200-500 nm, for example, 200 nm, 250 nm, 300 nm, 350 nm, 400 nm, 450 nm or 500 nm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0029] Preferably, the cathode electrochromic layer adopts a magnetron sputtering coating process, and the process parameters include: power 10 to 40 kW, for example, it can be 10 kW, 15 kW, 20 kW, 25 kW, 30 kW, 35 kW or 40 kW, but it is not limited to the listed values, and other values ​​not listed within the range are also applicable;

[0030] The coating temperature is 250-400°C, for example, it can be 250°C, 280°C, 300°C, 320°C, 350°C, 380°C or 400°C, but it is not limited to the listed values, and other values ​​not listed in the range are also applicable;

[0031] The coating pressure is 0.5 to 4.0 Pa, for example, it can be 0.5 Pa, 0.8 Pa, 1 Pa, 1.5 Pa, 2 Pa, 3 Pa or 4.0 Pa, but it is not limited to the listed values, and other values ​​not listed in the range are also applicable;

[0032] The argon gas flow rate is 200 to 1000 sccm, for example, it can be 200 sccm, 300 sccm, 400 sccm, 500 sccm, 600 sccm, 800 sccm or 1000 sccm, but is not limited to the listed values, and other values ​​not listed in the numerical range are also applicable;

[0033] The oxygen concentration is 20% to 100%, for example, it can be 20%, 30%, 40%, 50%, 60%, 80% or 100%, etc., but it is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable;

[0034] The coating speed is 0.1-1.0 m / min, for example, it can be 0.1 m / min, 0.3 m / min, 0.5 m / min, 0.8 m / min, 0.9 m / min, 0.95 m / min or 1.0 m / min, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0035] Preferably, the thickness of the lithium dielectric layer is 20 to 100 nm, for example, 20 nm, 25 nm, 30 nm, 50 nm, 70 nm, 90 nm or 100 nm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0036] Preferably, the lithium dielectric layer is coated by a magnetron sputtering process, and the process parameters include: power 2 to 15 kW, for example, 2 kW, 3 kW, 5 kW, 8 kW, 10 kW, 12 kW or 15 kW, etc., but are not limited to the listed values, and other values ​​not listed within the range are also applicable;

[0037] The coating temperature is 20 to 80° C., for example, it can be 20° C., 30° C., 50° C., 55° C., 60° C., 70° C. or 80° C., but is not limited to the listed values, and other values ​​not listed within the range are also applicable;

[0038] The coating pressure is 0.1-1.0 Pa, for example, it can be 0.1 Pa, 0.3 Pa, 0.4 Pa, 0.5 Pa, 0.6 Pa, 0.8 Pa or 1.0 Pa, etc., but it is not limited to the listed values, and other values ​​not listed in the range are also applicable;

[0039] The argon gas flow rate is 100 to 1000 sccm, for example, it can be 100 sccm, 200 sccm, 300 sccm, 500 sccm, 700 sccm, 900 sccm or 1000 sccm, but is not limited to the listed values, and other values ​​not listed in the numerical range are also applicable;

[0040] The coating speed is 0.1-1.0 m / min, for example, it can be 0.1 m / min, 0.3 m / min, 0.5 m / min, 0.8 m / min, 0.9 m / min, 0.95 m / min or 1.0 m / min, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0041] Preferably, the ion conducting layer comprises SiO2.

[0042] Preferably, the thickness of the ion conducting layer is 15 to 50 nm, for example, 15 nm, 20 nm, 25 nm, 30 nm, 35 nm, 40 nm or 50 nm, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0043] Preferably, the ion conductive layer is coated by a magnetron sputtering process, and the process parameters include: power 5 to 20 kW, for example, 5 kW, 6 kW, 8 kW, 10 kW, 12 kW, 15 kW or 20 kW, etc., but not limited to the listed values, and other values ​​not listed within the range are also applicable;

[0044] The coating temperature is 20 to 80° C., for example, it can be 20° C., 30° C., 40° C., 50° C., 60° C., 70° C. or 80° C., but is not limited to the listed values, and other values ​​not listed within the range are also applicable;

[0045] The coating pressure is 0.1-1.0 Pa, for example, it can be 0.1 Pa, 0.3 Pa, 0.5 Pa, 0.8 Pa, 0.9 Pa, 0.95 Pa or 1.0 Pa, etc., but it is not limited to the listed values, and other values ​​not listed in the range are also applicable;

[0046] The argon gas flow rate is 100 to 1000 sccm, for example, it can be 100 sccm, 200 sccm, 300 sccm, 500 sccm, 700 sccm, 900 sccm or 1000 sccm, but is not limited to the listed values, and other values ​​not listed in the numerical range are also applicable;

[0047] The oxygen concentration is 50% to 100%, for example, it can be 50%, 55%, 60%, 70%, 80%, 90% or 100%, etc., but it is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable;

[0048] The coating speed is 0.1-1.0 m / min, for example, it can be 0.1 m / min, 0.3 m / min, 0.5 m / min, 0.8 m / min, 0.9 m / min, 0.95 m / min or 1.0 m / min, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0049] Preferably, the anode electrochromic layer comprises NiWO x .

[0050] Preferably, the thickness of the anode electrochromic layer is 200-500 nm, for example, 200 nm, 250 nm, 300 nm, 350 nm, 400 nm, 450 nm or 500 nm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0051] Preferably, the anode electrochromic layer adopts a magnetron sputtering coating process, and the process parameters include: power 10 to 40 kW, for example, it can be 10 kW, 15 kW, 20 kW, 25 kW, 28 kW, 30 kW or 40 kW, but it is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable;

[0052] The coating temperature is 20 to 80° C., for example, it can be 20° C., 30° C., 50° C., 60° C., 65° C., 70° C. or 80° C., but is not limited to the listed values. Other values ​​not listed within the range are also applicable.

[0053] The coating pressure is 0.5 to 4.0 Pa, for example, it can be 0.5 Pa, 0.8 Pa, 1 Pa, 1.5 Pa, 2 Pa, 3 Pa or 4.0 Pa, but it is not limited to the listed values, and other values ​​not listed in the range are also applicable;

[0054] The argon gas flow rate is 200 to 1000 sccm, for example, it can be 200 sccm, 300 sccm, 400 sccm, 500 sccm, 600 sccm, 800 sccm or 1000 sccm, but is not limited to the listed values, and other values ​​not listed in the numerical range are also applicable;

[0055] The oxygen concentration is 20% to 100%, for example, it can be 20%, 30%, 40%, 50%, 60%, 80% or 100%, etc., but it is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable;

[0056] The coating speed is 0.1-1.0 m / min, for example, it can be 0.1 m / min, 0.3 m / min, 0.5 m / min, 0.8 m / min, 0.9 m / min, 0.95 m / min or 1.0 m / min, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0057] Preferably, the second transparent conductive layer comprises ITO conductive glass;

[0058] Preferably, the thickness of the second transparent conductive layer is 300-800 nm, for example, 300 nm, 350 nm, 400 nm, 500 nm, 600 nm, 700 nm or 800 nm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0059] Preferably, the second transparent conductive layer is coated by a magnetron sputtering process, and the process parameters include: power 2 to 10 kW, for example, 2 kW, 3 kW, 5 kW, 6 kW, 7 kW, 8 kW or 10 kW, etc., but are not limited to the listed values, and other values ​​not listed within the range are also applicable;

[0060] The coating temperature is 20 to 80° C., for example, it can be 20° C., 30° C., 50° C., 55° C., 60° C., 70° C. or 80° C., but is not limited to the listed values, and other values ​​not listed within the range are also applicable;

[0061] The coating pressure is 0.1-1.0 Pa, for example, it can be 0.1 Pa, 0.3 Pa, 0.4 Pa, 0.5 Pa, 0.6 Pa, 0.8 Pa or 1.0 Pa, etc., but it is not limited to the listed values, and other values ​​not listed in the range are also applicable;

[0062] The argon gas flow rate is 100 to 500 sccm, for example, 100 sccm, 150 sccm, 200 sccm, 300 sccm, 400 sccm, 450 sccm or 500 sccm, etc., but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable;

[0063] Oxygen concentration 0.1% to 1%, for example, can be 0.1%, 0.2%, 0.3%, 0.5%, 0.7%, 0.9% or 1%, etc., but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable;

[0064] The coating speed is 0.1-1.0 m / min, for example, it can be 0.1 m / min, 0.3 m / min, 0.5 m / min, 0.8 m / min, 0.9 m / min, 0.95 m / min or 1.0 m / min, etc., but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0065] Preferably, the pressure in the vacuum chamber during the vacuum baking process is 10 -2 ~10 -5 Pa, for example, can be 10 - 2 Pa, 10 -3 Pa, 10 -4 Pa or 10 -5 Pa, etc., but are not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0066] As a preferred technical solution of the present invention, the preparation method comprises the following steps:

[0067] In a vacuum chamber, after vacuum plating an electrochromic thin film layer on a glass substrate, vacuum baking is performed at a temperature of 200 to 400° C. for 30 to 120 minutes to obtain the electrochromic thin film product;

[0068] The electrochromic thin film layer comprises a first transparent conductive layer, a cathode electrochromic layer, a lithium dielectric layer, an ion conduction layer, an anode electrochromic layer and a second transparent conductive layer which are sequentially arranged from the glass substrate outward;

[0069] The first transparent conductive layer includes ITO conductive glass; the thickness of the first transparent conductive layer is 300-800nm; the first transparent conductive layer adopts a magnetron sputtering coating process, and the process parameters include: power 2-10kW, coating temperature 230-350°C, coating pressure 0.1-1.0Pa, argon flow rate 100-500sccm, oxygen concentration 0.1%-1%, and coating speed 0.1-1.0m / min;

[0070] The cathode electrochromic layer includes WO x ; The thickness of the cathode electrochromic layer is 200-500nm; the cathode electrochromic layer adopts a magnetron sputtering coating process, and the process parameters include: power 10-40kW, coating temperature 250-400°C, coating pressure 0.5-4.0Pa, argon flow rate 200-1000sccm, oxygen concentration 20%-100%, and coating speed 0.1-1.0m / min;

[0071] The thickness of the lithium dielectric layer is 20-100 nm; the lithium dielectric layer is coated by magnetron sputtering, and the process parameters include: power 2-15 kW, coating temperature 20-80° C., coating pressure 0.1-1.0 Pa, argon gas flow rate 100-1000 sccm, and coating speed 0.1-1.0 m / min;

[0072] The ion conductive layer comprises SiO2; the thickness of the ion conductive layer is 15-50 nm; the ion conductive layer is coated by magnetron sputtering, and the process parameters include: power 5-20 kW, coating temperature 20-80° C., coating pressure 0.1-1.0 Pa, argon flow rate 100-1000 sccm, oxygen concentration 50%-100%, and coating speed 0.1-1.0 m / min;

[0073] The anode electrochromic layer includes NiWO x ; The thickness of the anode electrochromic layer is 200-500nm; the anode electrochromic layer adopts a magnetron sputtering coating process, and the process parameters include: power 10-40kW, coating temperature 20-80°C, coating pressure 0.5-4.0Pa, argon flow rate 200-1000sccm, oxygen concentration 20%-100%, coating speed 0.1-1.0m / min;

[0074] The second transparent conductive layer includes ITO conductive glass; the thickness of the second transparent conductive layer is 300-800nm; the second transparent conductive layer adopts a magnetron sputtering coating process, and the process parameters include: power 2-10kW, coating temperature 20-80°C, coating pressure 0.1-1.0Pa, argon flow rate 100-500sccm, oxygen concentration 0.1%-1%, and coating speed 0.1-1.0m / min;

[0075] The pressure in the vacuum chamber during the vacuum baking process is 10 -2 ~10 -5 Pa.

[0076] In a second aspect, the present invention further provides an electrochromic thin film product, which is obtained by the preparation method of the electrochromic thin film product described in the first aspect.

[0077] The electrochromic thin film product of the present invention is vacuum coated and vacuum baked in a vacuum chamber, and does not require vacuum coating equipment, thereby avoiding contact between the product and external water vapor and dust, and the electrochromic thin film product has high quality.

[0078] In a third aspect, the present invention further provides an electrochromic thin film product as described in the second aspect for assembling an electrochromic device.

[0079] Compared with the prior art, the present invention has at least the following beneficial effects:

[0080] The preparation method of the electrochromic thin film product provided by the present invention does not require the product to leave the vacuum cavity during the preparation process, and the product will not be affected by external water vapor, dust, etc., which effectively improves the appearance quality of the product, and does not require specific vacuum baking treatment equipment, thereby reducing the preparation cost of the electrochromic thin film product. BRIEF DESCRIPTION OF THE DRAWINGS

[0081] Figure 1 This is a flow chart of the method for preparing the electrochromic thin film product provided in Example 1 of the present invention.

[0082] Figure 2 It is a schematic diagram of the structure of the electrochromic thin film product in Example 1 of the present invention.

[0083] Figure 3 It is a flow chart of the preparation method of the electrochromic thin film product provided in Comparative Example 1 of the present invention.

[0084] In the figure: 1-glass substrate; 2-first transparent conductive layer; 3-cathode electrochromic layer; 4-lithium dielectric layer; 5-ion conductive layer; 6-anode electrochromic layer; 7-second transparent conductive layer. DETAILED DESCRIPTION

[0085] The technical solution of the present invention is further described below with reference to the accompanying drawings and through specific implementation methods.

[0086] The present invention is further described in detail below. However, the following examples are only simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention shall be subject to the claims.

[0087] It should be understood that, in the description of the present invention, the terms "first", "second", etc. are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Thus, a feature defined as "first", "second", etc. may explicitly or implicitly include one or more of the features. In the description of the present invention, unless otherwise specified, "plurality" means two or more.

[0088] Example 1

[0089] This embodiment provides a method for preparing an electrochromic thin film product, and its flow chart is as follows: Figure 1 As shown, the preparation method comprises the following steps:

[0090] In a vacuum chamber, after vacuum plating the electrochromic thin film layer on the glass substrate, a vacuum baking treatment at a temperature of 200° C. for 30 minutes is performed to obtain the electrochromic thin film product, the structural schematic diagram of which is shown in FIG. Figure 2 As shown;

[0091] The electrochromic thin film layer comprises a first transparent conductive layer, a cathode electrochromic layer, a lithium dielectric layer, an ion conduction layer, an anode electrochromic layer and a second transparent conductive layer which are sequentially arranged from the glass substrate outward;

[0092] The first transparent conductive layer is ITO conductive glass; the thickness of the first transparent conductive layer is 500nm; the first transparent conductive layer adopts a magnetron sputtering coating process, and the process parameters include: power 3kW, coating temperature 250°C, coating pressure 0.4Pa, argon flow rate 170sccm, oxygen concentration 0.8%, and coating speed 0.6m / min;

[0093] The cathode electrochromic layer is WO x ; The thickness of the cathode electrochromic layer is 400nm; the cathode electrochromic layer adopts a magnetron sputtering coating process, and the process parameters include: power 16kW, coating temperature 290°C, coating pressure 0.7Pa, argon flow rate 500sccm, oxygen concentration 40%, coating speed 0.7m / min;

[0094] The thickness of the lithium dielectric layer is 60 nm; the lithium dielectric layer is coated by magnetron sputtering, and the process parameters include: power 10 kW, coating temperature 80° C., coating pressure 1.0 Pa, argon gas flow rate 600 sccm, and coating speed 0.1 m / min;

[0095] The ion conductive layer is SiO2; the thickness of the ion conductive layer is 50nm; the ion conductive layer is coated by magnetron sputtering, and the process parameters include: power 5kW, coating temperature 80°C, coating pressure 1.0Pa, argon flow rate 1000sccm, oxygen concentration 100%, coating speed 1.0m / min;

[0096] The anode electrochromic layer is NiWO x; The thickness of the anode electrochromic layer is 300nm; the anode electrochromic layer adopts a magnetron sputtering coating process, and the process parameters include: power 40kW, coating temperature 80°C, coating pressure 2.0Pa, argon flow rate 400sccm, oxygen concentration 20%, coating speed 1.0m / min;

[0097] The second transparent conductive layer is ITO conductive glass; the thickness of the second transparent conductive layer is 800nm; the second transparent conductive layer adopts a magnetron sputtering coating process, and the process parameters include: power 10kW, coating temperature 80°C, coating pressure 1.0Pa, argon flow rate 500sccm, oxygen concentration 1%, and coating speed 1.0m / min;

[0098] The pressure in the vacuum chamber during the vacuum baking process is 10 -5 Pa.

[0099] Example 2

[0100] This embodiment provides a method for preparing an electrochromic thin film product. The preparation method is the same as that of Embodiment 1 except that the vacuum baking treatment time is 60 minutes.

[0101] Example 3

[0102] This embodiment provides a method for preparing an electrochromic thin film product. The preparation method is the same as that of Embodiment 1 except that the vacuum baking treatment time is 90 minutes.

[0103] Example 4

[0104] This embodiment provides a method for preparing an electrochromic thin film product. The preparation method is the same as that of Embodiment 1 except that the temperature of the vacuum baking treatment is 300° C.

[0105] Example 5

[0106] This embodiment provides a method for preparing an electrochromic thin film product. The preparation method is the same as that of Embodiment 1 except that the temperature of the vacuum baking treatment is 300° C. and the time is 60 min.

[0107] Example 6

[0108] This embodiment provides a method for preparing an electrochromic thin film product. The preparation method is the same as that of Embodiment 1 except that the temperature of the vacuum baking treatment is 300° C. and the time is 90 min.

[0109] Example 7

[0110] This embodiment provides a method for preparing an electrochromic thin film product. The preparation method is the same as that of Embodiment 1 except that the temperature of the vacuum baking treatment is 400° C.

[0111] Example 8

[0112] This embodiment provides a method for preparing an electrochromic thin film product. The preparation method is the same as that of Embodiment 1 except that the temperature of the vacuum baking treatment is 400° C. and the time is 60 min.

[0113] Example 9

[0114] This embodiment provides a method for preparing an electrochromic thin film product. The preparation method is the same as that of Embodiment 1 except that the temperature of the vacuum baking treatment is 400° C. and the time is 90 min.

[0115] Example 10

[0116] This embodiment provides a method for preparing an electrochromic thin film product. The preparation method is the same as that of Embodiment 1 except that the temperature of the vacuum baking treatment is 350° C. and the time is 60 min.

[0117] Comparative Example 1

[0118] This comparative example provides a method for preparing an electrochromic thin film product, and its flow chart is as follows Figure 3 The preparation method comprises the following steps:

[0119] After vacuum plating the electrochromic thin film layer on the glass substrate in a vacuum chamber, the product is taken out of the chamber and placed in an atmospheric baking device for vacuum baking at a temperature of 200° C. for 30 minutes to obtain the electrochromic thin film product; the preparation process parameters of the electrochromic thin film layer are the same as those in Example 1.

[0120] Comparative Example 2

[0121] This comparative example provides a method for preparing an electrochromic thin film product. The preparation method is the same as Example 1 except that the temperature of the vacuum baking treatment is 150° C.

[0122] Comparative Example 3

[0123] This comparative example provides a method for preparing an electrochromic thin film product. The preparation method is the same as Example 1 except that the temperature of the vacuum baking treatment is 450° C.

[0124] The transmittance of the electrochromic thin film products obtained in the above examples and comparative examples was measured using a transmittance measuring instrument, and the results are shown in Table 1 below.

[0125] Table 1

[0126] Transmittance Example 1 68.8％ Example 2 69.1％ Example 3 69.6％ Example 4 69.3％ Example 5 70.0％ Example 6 71.1％ Example 7 68.5％ Example 8 70.6％ Example 9 71.8％ Example 10 71.1％ Comparative Example 1 71.8％ Comparative Example 2 34.5％ Comparative Example 3 56.3％

[0127] From Table 1 we can see that:

[0128] (1) It can be seen from Examples 1 to 10 that the preparation method of the electrochromic thin film product provided by the present invention directly performs vacuum baking after completing vacuum coating in a vacuum chamber, without the need for additional vacuum baking equipment, and has low preparation cost; the transmittance of the obtained electrochromic thin film product is between 68.8% and 71.8%, which meets the use requirements;

[0129] (2) Based on Example 9 and Comparative Example 1, it can be seen that the transmittance of the electrochromic thin film product obtained by directly performing vacuum baking treatment after vacuum coating in a vacuum chamber in Example 9 is equivalent to the transmittance of the electrochromic thin film product obtained by performing atmospheric baking treatment in an atmospheric baking device after coating in a vacuum chamber in the prior art of Comparative Example 1; and Example 9 does not require additional baking treatment equipment, and the preparation cost is lower than that of Comparative Example 1;

[0130] (3) Based on Example 1 and Comparative Examples 2 to 3, it can be seen that the vacuum baking treatment temperature of Comparative Example 2 is relatively low, while the vacuum baking treatment temperature of Comparative Example 3 is relatively high, both of which will lead to attenuation of the transmittance of the final electrochromic film product, affecting the subsequent use effect.

[0131] The applicant declares that the above is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention shall fall within the protection scope and disclosure scope of the present invention.

Claims

1. A method for preparing an electrochromic thin film product, characterized in that: The preparation method comprises the following steps: In a vacuum chamber, after vacuum plating an electrochromic thin film layer on a glass substrate, vacuum baking is performed at a temperature of 200 to 400° C. for 30 to 120 minutes to obtain the electrochromic thin film product; The electrochromic thin film layer comprises a first transparent conductive layer, a cathode electrochromic layer, a lithium dielectric layer, an ion conduction layer, an anode electrochromic layer and a second transparent conductive layer which are sequentially arranged from a glass substrate outward.

2. The preparation method according to claim 1, characterized in that The first transparent conductive layer comprises ITO conductive glass; Preferably, the thickness of the first transparent conductive layer is 300-800 nm; Preferably, the first transparent conductive layer is coated by a magnetron sputtering process, and the process parameters include: power 2-10kW, coating temperature 230-350°C, coating pressure 0.1-1.0Pa, argon flow rate 100-500sccm, oxygen concentration 0.1%-1%, and coating speed 0.1-1.0m / min.

3. The preparation method according to claim 1 or 2, characterized in that: The cathode electrochromic layer includes WO x ; Preferably, the thickness of the cathode electrochromic layer is 200 to 500 nm; Preferably, the cathode electrochromic layer is coated by a magnetron sputtering process, and the process parameters include: power 10-40kW, coating temperature 250-400°C, coating pressure 0.5-4.0Pa, argon flow rate 200-1000sccm, oxygen concentration 20%-100%, and coating speed 0.1-1.0m / min.

4. The preparation method according to any one of claims 1 to 3, characterized in that: The thickness of the lithium dielectric layer is 20 to 100 nm; Preferably, the lithium dielectric layer is coated by a magnetron sputtering process, and the process parameters include: power 2-15 kW, coating temperature 20-80° C., coating pressure 0.1-1.0 Pa, argon gas flow rate 100-1000 sccm, and coating speed 0.1-1.0 m / min.

5. The preparation method according to any one of claims 1 to 4, characterized in that: The ion conducting layer comprises SiO2; Preferably, the thickness of the ion conducting layer is 15 to 50 nm; Preferably, the ion conductive layer is coated by a magnetron sputtering process, and the process parameters include: power 5-20kW, coating temperature 20-80°C, coating pressure 0.1-1.0Pa, argon flow rate 100-1000sccm, oxygen concentration 50%-100%, and coating speed 0.1-1.0m / min.

6. The preparation method according to any one of claims 1 to 5, characterized in that: The anode electrochromic layer includes NiWO x ; Preferably, the thickness of the anode electrochromic layer is 200-500 nm; Preferably, the anode electrochromic layer is coated by a magnetron sputtering process, and the process parameters include: power 10-40kW, coating temperature 20-80°C, coating pressure 0.5-4.0Pa, argon flow rate 200-1000sccm, oxygen concentration 20%-100%, and coating speed 0.1-1.0m / min.

7. The preparation method according to any one of claims 1 to 6, characterized in that: The second transparent conductive layer includes ITO conductive glass; Preferably, the thickness of the second transparent conductive layer is 300-800 nm; Preferably, the second transparent conductive layer is coated by a magnetron sputtering process, and the process parameters include: power 2-10kW, coating temperature 20-80°C, coating pressure 0.1-1.0Pa, argon flow rate 100-500sccm, oxygen concentration 0.1%-1%, and coating speed 0.1-1.0m / min.

8. The preparation method according to any one of claims 1 to 7, characterized in that: The pressure in the vacuum chamber during the vacuum baking process is 10 -2 ~10 -5 Pa.

9. An electrochromic thin film product, characterized in that: The electrochromic thin film product is obtained by the preparation method of the electrochromic thin film product according to any one of claims 1 to 8.

10. An electrochromic thin film product as claimed in claim 9 for assembling an electrochromic device.

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