Anti-short-circuit electrochromic film structure and preparation method thereof

Abstract

The invention provides an anti-short-circuit electrochromic film structure and a preparation method thereof. The anti-short-circuit electrochromic film structure comprises a substrate layer, and a first transparent conductive layer, an insulation isolation layer, a cathode electrochromic layer, a dielectric layer, an ion conduction layer, an anode electrochromic layer and a second transparent conductive layer are sequentially arranged on the substrate layer in an overlapped mode. By optimizing the film layer structure of the electrochromic product, the leakage current caused by short circuit of the electrochromic film layer is improved, and meanwhile the requirement for coloring time is further met.

Description

Technical Field

[0001] The present invention belongs to the technical field of electrochromic technology, and particularly relates to an anti-short-circuit electrochromic film structure and a preparation method thereof. Background Art

[0002] Electrochromic technology, relying on its unique optical properties, has been widely applied in multiple fields such as smart windows, electronic displays, and automotive rearview mirrors. By applying an external electric field, electrochromic products can achieve reversible changes in color and transmittance, meeting the diverse requirements for light and visual effects in different scenarios. However, during the production and application of electrochromic products, the problem of film layer short circuit seriously hinders the further improvement of their performance and market expansion.

[0003] Electrochromic products usually consist of multiple functional film layers, including an electrochromic layer, an ion conductor layer, a transparent conductive layer, etc. Each film layer needs to maintain good insulation and stability to ensure the normal functioning of the electrochromic function. However, during the actual preparation process, affected by various factors, short circuits are likely to occur between the film layers. On the one hand, in a high-temperature and high-humidity environment, some substances in the film layer may migrate or corrode, resulting in damage to the film layer structure, forming a conductive path in the originally insulated area, and thus triggering a short circuit. On the other hand, during the film coating process, if the process parameters are not properly controlled, such as uneven film coating thickness or the presence of impurity particles on the film layer surface, it will cause the film layer spacing to be too small or the film layer to peel off in local areas, providing an abnormal channel for the current and causing a short circuit failure.

[0004] Film layer short circuit brings many negative impacts to electrochromic products. From the perspective of performance, short circuit will slow down the electrochromic response speed, and the color change is not obvious, seriously affecting the optical performance of the product and reducing its use effect. In the application of smart windows, this will lead to the inability to adjust indoor light in a timely and effective manner, affecting the user experience. From the perspective of product life, the local overheating caused by short circuit will accelerate the aging of the film layer, significantly shortening the service life of the product and increasing the maintenance and replacement costs. In addition, short circuit may also cause safety hazards. For example, in scenarios with high safety requirements such as automotive rearview mirrors, short circuit may cause abnormal display of the rearview mirror, affecting the driver's line of sight and endangering driving safety.

[0005] At present, regarding the problem of short - circuit in the film layer of electrochromic products, there have been some studies and solutions. Some studies have tried to improve the corrosion resistance and insulation performance of the film layer by improving the film layer material, so as to reduce the short - circuit risk. However, the R & D cost of new materials is high, and in practical applications, the compatibility between new materials and existing production processes is poor, making it difficult to promote on a large scale. There are also some studies dedicated to optimizing the coating process, such as using more precise coating equipment and stricter process control to improve the uniformity and quality of the film layer. But these methods have strict requirements for equipment and processes, not only increasing the production cost, but also difficult to fundamentally solve the problem of film layer short - circuit caused by environmental factors.

[0006] In summary, the existing methods for solving the short - circuit problem of the film layer of electrochromic products have many deficiencies. Developing an efficient, low - cost and easy - to - implement solution and its preparation method has important practical significance for promoting the development of electrochromic technology, improving the performance and market competitiveness of electrochromic products. Summary of the Invention

[0007] Aiming at the deficiencies of the existing technology, the purpose of the present invention is to provide an anti - short - circuit electrochromic film structure and its preparation method. By setting an insulating isolation layer with excellent compactness and insulation, the present invention realizes the blocking of foreign particles between conductive layers, further avoiding the defect of short - circuit in electrochromic products.

[0008] To achieve the purpose of this invention, the following technical solutions are adopted:

[0009] In the first aspect, the present invention provides an anti - short - circuit electrochromic film structure, which includes a base layer, and a first transparent conductive layer, an insulating isolation layer, a cathode electrochromic layer, a dielectric layer, an ion - conducting layer, an anode electrochromic layer, and a second transparent conductive layer are sequentially stacked above the base layer.

[0010] Currently, during the preparation process of electrochromic film structures, foreign particles are generated during the film coating process, and some foreign particles will fall off under the influence of stress and other factors during the coating process of other film layers. The falling off of foreign particles brings the risk of short - circuit between the upper and lower transparent conductive layers;

[0011] In the present invention, the insulating isolation layer has excellent compactness and insulation, and has good adhesion on the surface of the first transparent conductive layer. By depositing the insulating isolation layer between the first transparent conductive layer and the cathode electrochromic layer, the blocking of falling foreign particles between the first transparent conductive layer and the second transparent conductive layer is realized, further avoiding abnormal film layer short - circuit.

[0012] It should be noted that when the first transparent conductive layer in the electrochromic film structure is connected to the negative electrode and the second transparent conductive layer is connected to the positive electrode, the electrochromic film structure exhibits a dark state; conversely, when the first transparent conductive layer is connected to the positive electrode and the second transparent conductive layer is connected to the negative electrode, the electrochromic film structure exhibits a transparent state.

[0013] As a preferred technical solution of the present invention, the material of the insulation isolation layer includes titanium oxide.

[0014] Preferably, the thickness of the insulation isolation layer is 5-30 nm, for example, it can be 5 nm, 10 nm, 15 nm, 20 nm, 25 nm or 30 nm, etc., but is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0015] Preferably, the refractive index of the insulation isolation layer is 2.3-2.5, for example, it can be 2.3, 2.34, 2.38, 2.42, 2.46 or 2.5, etc., but is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0016] In the present invention, the insulation isolation layer has excellent compactness, insulation and adhesion. If its thickness is too thick, the transmittance in the transparent state will become low and the color change speed will become slow. If the thickness is too thin, the insulation blocking effect will be poor and micro-short circuit will occur.

[0017] As a preferred technical solution of the present invention, the material of the base layer includes float glass.

[0018] Preferably, the thickness of the base layer is 0.4-5.0 mm, for example, it can be 0.4 mm, 1 mm, 2 mm, 3 mm, 4 mm or 5 mm, etc., but is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0019] As a preferred technical solution of the present invention, the first transparent conductive layer includes an ITO film layer.

[0020] Preferably, the material of the cathode electrochromic layer includes tungsten oxide.

[0021] Preferably, the dielectric layer includes a lithium layer.

[0022] Preferably, the material of the ion conduction layer includes silicon oxide or silicon aluminum oxide.

[0023] It should be noted that the atomic ratio of silicon to aluminum in the silicon aluminum oxide is 90-95:10-5, for example, it can be 90:10, 91:9, 92:8, 93:7, 94:6 or 95:5, etc., but is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0024] Preferably, the material of the anodic electrochromic layer includes nickel tungsten oxide.

[0025] It should be noted that the atomic ratio of tungsten to nickel in the nickel tungsten oxide is 50 - 55:45 - 50. For example, it can be 50:50, 52:48, 54:46, or 52:48, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0026] Preferably, the second transparent conductive layer includes an ITO film layer.

[0027] As a preferred technical solution of the present invention, the thickness of the first transparent conductive layer is 100 - 500 nm. For example, it can be 100 nm, 200 nm, 300 nm, 400 nm, or 500 nm, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0028] Preferably, the thickness of the cathodic electrochromic layer is 200 - 500 nm. For example, it can be 200 nm, 300 nm, 400 nm, or 500 nm, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0029] Preferably, the thickness of the dielectric layer is 100 - 300 nm. For example, it can be 100 nm, 150 nm, 200 nm, 250 nm, or 300 nm, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0030] Preferably, the thickness of the ion conduction layer is 5 - 25 nm. For example, it can be 5 nm, 10 nm, 15 nm, 20 nm, or 25 nm, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0031] Preferably, the thickness of the anodic electrochromic layer is 200 - 500 nm. For example, it can be 200 nm, 300 nm, 400 nm, or 500 nm, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0032] Preferably, the thickness of the second transparent conductive layer is 300 - 900 nm. For example, it can be 300 nm, 400 nm, 500 nm, 700 nm, or 900 nm, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0033] In a second aspect, the present invention provides a method for preparing the short - circuit - proof electrochromic film structure as described in the first aspect. The preparation method includes:

[0034] By using the method of vacuum magnetron sputtering coating, a first transparent conductive layer, an insulating isolation layer, a cathode electrochromic layer, a dielectric layer, an ion conduction layer, an anode electrochromic layer, and a second transparent conductive layer are sequentially coated above the base layer.

[0035] As a preferred technical solution of the present invention, the coating speed during the coating process is 0.1 - 1 m / min. For example, it can be 0.1 m / min, 0.3 m / min, 0.5 m / min, 0.8 m / min, or 1 m / min, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0036] As a preferred technical solution of the present invention, during the process of coating the insulating isolation layer, the power density of magnetron sputtering is 5 - 15 kw / m. For example, it can be 5 kw / m, 8 kw / m, 11 kw / m, or 15 kw / m, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0037] Preferably, during the process of coating the insulating isolation layer, the coating temperature of magnetron sputtering is 250 - 400 °C. For example, it can be 250 °C, 300 °C, 350 °C, or 400 °C, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0038] Preferably, during the process of coating the insulating isolation layer, the coating pressure of magnetron sputtering is 0.1 - 1 Pa. For example, it can be 0.1 Pa, 0.3 Pa, 0.5 Pa, 0.8 Pa, or 1 Pa, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0039] Preferably, during the process of coating the insulating isolation layer, the gas for magnetron sputtering includes oxygen and argon.

[0040] Preferably, during the process of coating the insulating isolation layer, the oxygen flow rate of magnetron sputtering is 20 - 80% of the total gas flow rate. For example, it can be 20%, 40%, 60%, or 80%, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0041] Preferably, during the process of coating the insulating isolation layer, the argon flow rate in magnetron sputtering is 100 - 1000 sccm. For example, it can be 100 sccm, 300 sccm, 500 sccm, 700 sccm, or 1000 sccm, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0042] The present invention realizes the improvement of the density and adsorption force of the insulating isolation layer by optimizing the process parameters during the plating process. If the temperature during the plating process is too high, it will cause fragmentation, and if the temperature is too low, the insulation of the film will deteriorate.

[0043] As a preferred technical solution of the present invention, during the plating of the first transparent conductive layer, the power density of magnetron sputtering is 2-6 kw / m, for example, it can be 2 kw / m, 3 kw / m, 4 kw / m, 5 kw / m or 6 kw / m, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0044] Preferably, during the plating of the first transparent conductive layer, the coating temperature of magnetron sputtering is 230-350 °C, for example, it can be 230 °C, 250 °C, 290 °C, 320 °C or 350 °C, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0045] Preferably, during the plating of the first transparent conductive layer, the coating pressure of magnetron sputtering is 0.1-1.0 Pa, for example, it can be 0.1 Pa, 0.3 Pa, 0.5 Pa, 0.8 Pa or 1 Pa, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0046] Preferably, during the plating of the first transparent conductive layer, the gas for magnetron sputtering includes oxygen and argon.

[0047] Preferably, during the plating of the first transparent conductive layer, the oxygen flow rate of magnetron sputtering is 0.1-1% of the total gas flow rate, for example, it can be 0.1%, 0.3%, 0.5%, 0.8% or 1%, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0048] Preferably, during the plating of the first transparent conductive layer, the argon flow rate in magnetron sputtering is 100-500 sccm, for example, it can be 100 sccm, 200 sccm, 300 sccm, 400 sccm or 500 sccm, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0049] As a preferred technical solution of the present invention, during the plating of the cathode electrochromic layer, the power density of magnetron sputtering is 10-20 kw / m, for example, it can be 10 kw / m, 12 kw / m, 14 kw / m, 16 kw / m, 18 kw / m or 20 kw / m, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0050] Preferably, during the deposition of the cathode electrochromic layer, the coating temperature of magnetron sputtering is 250 to 400 °C. For example, it can be 250 °C, 300 °C, 350 °C, or 400 °C, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0051] Preferably, during the deposition of the cathode electrochromic layer, the coating pressure of magnetron sputtering is 0.5 to 4.0 Pa. For example, it can be 0.5 Pa, 1 Pa, 2 Pa, 3 Pa, or 4 Pa, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0052] Preferably, during the deposition of the cathode electrochromic layer, the magnetron sputtering gas includes oxygen and argon.

[0053] Preferably, during the deposition of the cathode electrochromic layer, the oxygen flow rate in magnetron sputtering is 20 to 100% of the total gas flow rate. For example, it can be 20%, 40%, 60%, 80%, or 100%, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0054] Preferably, during the deposition of the cathode electrochromic layer, the argon flow rate in magnetron sputtering is 200 to 1000 sccm. For example, it can be 200 sccm, 400 sccm, 600 sccm, 800 sccm, or 1000 sccm, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0055] As a preferred technical solution of the present invention, during the deposition of the dielectric layer, the power density in magnetron sputtering is 2 to 10 kw / m. For example, it can be 2 kw / m, 4 kw / m, 6 kw / m, 8 kw / m, or 10 kw / m, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0056] Preferably, during the deposition of the dielectric layer, the coating temperature of magnetron sputtering is 20 to 80 °C. For example, it can be 20 °C, 40 °C, 60 °C, or 80 °C, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0057] Preferably, during the deposition of the dielectric layer, the coating pressure of magnetron sputtering is 0.1 to 1 Pa. For example, it can be 0.1 Pa, 0.3 Pa, 0.5 Pa, 0.7 Pa, or 1 Pa, etc., but not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0058] Preferably, during the deposition of the dielectric layer, the argon flow rate in magnetron sputtering is 100 - 1000 sccm. For example, it can be 100 sccm, 300 sccm, 500 sccm, 700 sccm, 1000 sccm, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0059] As a preferred technical solution of the present invention, during the deposition of the ion conduction layer, the power density in magnetron sputtering is 5 - 12 kw / m². For example, it can be 5 kw / m², 7 kw / m², 9 kw / m², 12 kw / m², etc., but is not limited to the listed values. Values within the numerical range are equally applicable.

[0060] Preferably, during the deposition of the ion conduction layer, the coating temperature in magnetron sputtering is 20 - 80 °C. For example, it can be 20 °C, 40 °C, 60 °C, 80 °C, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0061] Preferably, during the deposition of the ion conduction layer, the coating pressure in magnetron sputtering is 0.1 - 1 Pa. For example, it can be 0.1 Pa, 0.3 Pa, 0.5 Pa, 0.7 Pa, 1 Pa, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0062] Preferably, during the deposition of the ion conduction layer, the gases in magnetron sputtering include oxygen and argon.

[0063] Preferably, during the deposition of the ion conduction layer, the oxygen flow rate in magnetron sputtering is 65 - 100% of the total gas flow rate. For example, it can be 65%, 70%, 80%, 90%, 100%, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0064] Preferably, during the deposition of the ion conduction layer, the argon flow rate in magnetron sputtering is 200 - 1000 sccm. For example, it can be 200 sccm, 500 sccm, 700 sccm, 1000 sccm, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0065] As a preferred technical solution of the present invention, during the deposition of the anode electrochromic layer, the power density in magnetron sputtering is 10 - 20 kw / m². For example, it can be 10 kw / m², 13 kw / m², 17 kw / m², 20 kw / m², etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0066] Preferably, during the deposition of the anode electrochromic layer, the coating temperature of magnetron sputtering is 20 to 80 °C, for example, it can be 20 °C, 40 °C, 60 °C or 80 °C, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0067] Preferably, during the deposition of the anode electrochromic layer, the coating pressure of magnetron sputtering is 0.5 to 4 Pa, for example, it can be 0.5 Pa, 1 Pa, 2 Pa, 3 Pa or 4 Pa, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0068] Preferably, during the deposition of the anode electrochromic layer, the magnetron sputtering gas includes oxygen and argon.

[0069] Preferably, during the deposition of the anode electrochromic layer, the flow rate of oxygen during magnetron sputtering is 20 to 100% of the total gas flow rate, for example, it can be 20%, 40%, 60%, 80% or 100%, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0070] Preferably, during the deposition of the anode electrochromic layer, the argon flow rate of magnetron sputtering is 200 to 1000 sccm, for example, it can be 200 sccm, 500 sccm, 700 sccm or 1000 sccm, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0071] As a preferred technical solution of the present invention, during the deposition of the second transparent conductive layer, the power density of magnetron sputtering is 2 to 6 kw / m, for example, it can be 2 kw / m, 3 kw / m, 4 kw / m, 5 kw / m or 6 kw / m, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0072] Preferably, during the deposition of the second transparent conductive layer, the coating temperature of magnetron sputtering is 20 to 80 °C, for example, it can be 20 °C, 40 °C, 60 °C or 80 °C, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0073] Preferably, during the deposition of the second transparent conductive layer, the coating pressure of magnetron sputtering is 0.1 to 1 Pa, for example, it can be 0.1 Pa, 0.3 Pa, 0.5 Pa, 0.7 Pa or 1 Pa, etc., but not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0074] Preferably, during the deposition of the second transparent conductive layer, the magnetron sputtering gas includes oxygen and argon.

[0075] Preferably, during the deposition of the second transparent conductive layer, the oxygen flow rate in magnetron sputtering is 0.1-1% of the total gas flow rate. For example, it can be 0.1%, 0.3%, 0.5%, 0.75% or 1%, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0076] Preferably, during the deposition of the second transparent conductive layer, the argon flow rate in magnetron sputtering is 200-500 sccm. For example, it can be 200 sccm, 300 sccm, 400 sccm or 500 sccm, etc., but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0077] As a preferred technical solution of the present invention, the preparation method of the short-circuit-proof electrochromic film structure of the present invention includes:

[0078] Using the method of vacuum magnetron sputtering coating, the first transparent conductive layer, the insulating isolation layer, the cathode electrochromic layer, the dielectric layer, the ion conduction layer, the anode electrochromic layer and the second transparent conductive layer are sequentially deposited above the base layer at a deposition rate of 0.1-1 m / min;

[0079] Among them, during the deposition of the first transparent conductive layer, the power density of magnetron sputtering is 2-6 kw / m, the coating temperature is 230-350 °C, the coating pressure is 0.1-1.0 Pa, the oxygen flow rate is 0.1-1% of the total gas flow rate, and the argon flow rate is 100-500 sccm;

[0080] During the deposition of the insulating isolation layer, the power density of magnetron sputtering is 5-15 kw / m, the coating temperature is 250-400 °C, the coating pressure is 0.1-1 Pa; the gas includes oxygen and argon, the oxygen flow rate is 20-80% of the total gas flow rate, and the oxygen flow rate is 20-80% of the total gas flow rate;

[0081] During the deposition of the cathode electrochromic layer, the power density of magnetron sputtering is 10-20 kw / m, the coating temperature is 250-400 °C, the coating pressure is 0.5-4.0 Pa, the oxygen flow rate is 20-100% of the total gas flow rate, and the argon flow rate is 200-1000 sccm;

[0082] During the deposition of the dielectric layer, the power density during magnetron sputtering is 2-10 kw / m, the coating temperature is 20-80 °C, the coating pressure is 0.1-1 Pa, and the argon flow rate is 100-1000 sccm;

[0083] During the deposition of the ion conduction layer, the power density of magnetron sputtering is 5-12 kw / m, the coating temperature is 20-80 °C, the coating pressure is 0.1-1 Pa, the oxygen flow rate is 65-100% of the total gas flow rate, and the argon flow rate is 200-1000 sccm;

[0084] During the deposition of the anode electrochromic layer, the power density of magnetron sputtering is 10-20 kw / m, the coating temperature is 20-80 °C, the coating pressure is 0.5-4 Pa, the oxygen flow rate is 20-100% of the total gas flow rate, and the argon flow rate is 200-1000 sccm;

[0085] During the deposition of the second transparent conductive layer, the power density of magnetron sputtering is 2-6 kw / m, the coating temperature is 20-80 °C, the coating pressure is 0.1-1 Pa, the oxygen flow rate is 0.1-1% of the total gas flow rate, and the argon flow rate is 200-500 sccm.

[0086] The numerical ranges described in the present invention include not only the point values exemplified above, but also any point values between the above numerical ranges not exemplified. Due to space limitations and for the sake of brevity, the present invention does not exhaustively list the specific point values included in the described ranges.

[0087] Compared with the prior art, the present invention has the following beneficial effects:

[0088] (1) By providing an insulating isolation layer with excellent denseness and insulation, the present invention realizes the blocking of foreign particles between conductive layers, and further avoids the defect of short circuit in electrochromic products;

[0089] (2) The leakage current of the electrochromic product including the short-circuit prevention electrochromic film structure provided by the present invention can be as low as about 5 μA / cm 2 or so, and the coloring time is as low as 750 s, realizing a significant improvement in product performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0090] Figure 1 is a schematic structural diagram of the short-circuit prevention electrochromic film structure provided in Embodiment 1 of the present invention;

[0091] Among them, 1 is the base layer, 2 is the first transparent conductive layer, 3 is the insulating isolation layer, 4 is the cathode electrochromic layer, 5 is the dielectric layer, 6 is the ion conduction layer, 7 is the anode electrochromic layer, and 8 is the second transparent conductive layer. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0092] The technical solutions of the present invention will be further described below through specific embodiments. Those skilled in the art should understand that the described embodiments are only for helping to understand the present invention and should not be regarded as specific limitations on the present invention.

[0093] Example 1

[0094] This example provides a short - circuit - proof electrochromic film structure, as Figure 1 shown. The short - circuit - proof electrochromic film structure includes a base layer 1, and a first transparent conductive layer 2, an insulating isolation layer 3, a cathode electrochromic layer 4, a dielectric layer 5, an ion - conducting layer 6, an anode electrochromic layer 7, and a second transparent conductive layer 8 are sequentially stacked above the base layer 1.

[0095] The insulating isolation layer 3 is made of titanium oxide, with a thickness of 20 nm and a refractive index of 2.4;

[0096] The base layer 1 is made of float glass, with a thickness of 2.5 mm;

[0097] The first transparent conductive layer 2 is an ITO film layer; with a thickness of 300 nm;

[0098] The cathode electrochromic layer 4 is made of tungsten oxide; with a thickness of 350 nm;

[0099] The dielectric layer 5 is a lithium layer; with a thickness of 200 nm;

[0100] The ion - conducting layer 6 is made of silicon oxide; with a thickness of 15 nm;

[0101] The anode electrochromic layer 7 is made of tungsten nickel oxide; with a thickness of 350 nm;

[0102] The second transparent conductive layer 8 is an ITO film layer; with a thickness of 600 nm.

[0103] The preparation method of the short - circuit - proof electrochromic film structure includes:

[0104] Using the method of vacuum magnetron sputtering coating, the first transparent conductive layer, insulating isolation layer, cathode electrochromic layer, dielectric layer, ion - conducting layer, anode electrochromic layer, and the second transparent conductive layer are sequentially coated above the base layer at a coating speed of 0.5 m / min;

[0105] Among them, during the coating process of the first transparent conductive layer, the power density of magnetron sputtering is 4 kw / m, the coating temperature is 300 °C, the coating pressure is 0.5 Pa, the oxygen flow rate is 0.5% of the total gas flow rate, and the argon flow rate is 300 sccm;

[0106] During the coating process of the insulating isolation layer, the power density of magnetron sputtering is 14 kw / m, the coating temperature is 350 °C, the coating pressure is 0.5 Pa; the gas includes oxygen and argon, the oxygen flow rate is 60% of the total gas flow rate, and the argon flow rate is 550 sccm;

[0107] During the deposition of the cathode electrochromic layer, the power density of magnetron sputtering is 15 kw / m, the coating temperature is 300 °C, the coating pressure is 2.5 Pa, the oxygen flow rate is 40% of the total gas flow rate, and the argon flow rate is 600 sccm;

[0108] During the deposition of the dielectric layer, the power density during magnetron sputtering is 6 kw / m, the coating temperature is 60 °C, the coating pressure is 0.2 Pa, and the argon flow rate is 200 sccm;

[0109] During the deposition of the ion-conducting layer, the power density of magnetron sputtering is 5 kw / m, the coating temperature is 80 °C, the coating pressure is 0.1 Pa, the oxygen flow rate is 80% of the total gas flow rate, and the argon flow rate is 200 sccm;

[0110] During the deposition of the anode electrochromic layer, the power density of magnetron sputtering is 20 kw / m, the coating temperature is 20 °C, the coating pressure is 2.4 Pa, the oxygen flow rate is 60% of the total gas flow rate, and the argon flow rate is 700 sccm;

[0111] During the deposition of the second transparent conductive layer, the power density of magnetron sputtering is 4 kw / m, the coating temperature is 30 °C, the coating pressure is 0.1 Pa, the oxygen flow rate is 0.7% of the total gas flow rate, and the argon flow rate is 400 sccm.

[0112] Example 2

[0113] This example provides a short-circuit-proof electrochromic film structure, as Figure 1 shown. The short-circuit-proof electrochromic film structure includes a base layer 1, and a first transparent conductive layer 2, an insulating isolation layer 3, a cathode electrochromic layer 4, a dielectric layer 5, an ion-conducting layer 6, an anode electrochromic layer 7, and a second transparent conductive layer 8 are sequentially stacked above the base layer 1.

[0114] The insulating isolation layer 3 is made of titanium oxide, with a thickness of 5 nm and a refractive index of 2.3;

[0115] The base layer 1 is made of float glass, with a thickness of 5.0 mm;

[0116] The first transparent conductive layer 2 is an ITO film layer; with a thickness of 100 nm;

[0117] The cathode electrochromic layer 4 is made of tungsten oxide; with a thickness of 200 nm;

[0118] The dielectric layer 5 is a lithium layer; with a thickness of 100 nm;

[0119] The ion-conducting layer 6 is made of silicon aluminum oxide; with a thickness of 5 nm;

[0120] The material of the anode electrochromic layer 7 is nickel tungsten oxide; the thickness is 200 nm;

[0121] The second transparent conductive layer 8 is an ITO film layer; the thickness is 300 nm.

[0122] The preparation method of the short - circuit prevention electrochromic film structure includes:

[0123] Adopt the method of vacuum magnetron sputtering coating, and sequentially coat the first transparent conductive layer, insulating isolation layer, cathode electrochromic layer, dielectric layer, ion conduction layer, anode electrochromic layer and the second transparent conductive layer above the substrate layer at a coating speed of 0.1 m / min;

[0124] Among them, during the coating process of the first transparent conductive layer, the power density of magnetron sputtering is 2 kw / m, the coating temperature is 350 °C, the coating pressure is 1.0 Pa, the oxygen flow rate is 0.1% of the total gas flow rate, and the argon flow rate is 100 sccm;

[0125] During the coating process of the insulating isolation layer, the power density of magnetron sputtering is 15 kw / m, the coating temperature is 250 °C, the coating pressure is 1 Pa; the gas includes oxygen and argon, the oxygen flow rate is 40% of the total gas flow rate, and the argon flow rate is 400 sccm;

[0126] During the coating process of the cathode electrochromic layer, the power density of magnetron sputtering is 20 kw / m, the coating temperature is 400 °C, the coating pressure is 0.5 Pa, the oxygen flow rate is 60% of the total gas flow rate, and the argon flow rate is 1000 sccm;

[0127] During the coating process of the dielectric layer, the power density during magnetron sputtering is 8 kw / m, the coating temperature is 40 °C, the coating pressure is 0.3 Pa, and the argon flow rate is 400 sccm;

[0128] During the coating process of the ion conduction layer, the power density of magnetron sputtering is 10 kw / m, the coating temperature is 60 °C, the coating pressure is 0.6 Pa, the oxygen flow rate is 70% of the total gas flow rate, and the argon flow rate is 400 sccm;

[0129] During the coating process of the anode electrochromic layer, the power density of magnetron sputtering is 10 kw / m, the coating temperature is 80 °C, the coating pressure is 4 Pa, the oxygen flow rate is 20% of the total gas flow rate, and the argon flow rate is 200 sccm;

[0130] During the coating process of the second transparent conductive layer, the power density of magnetron sputtering is 2 kw / m, the coating temperature is 20 °C, the coating pressure is 1 Pa, the oxygen flow rate is 1% of the total gas flow rate, and the argon flow rate is 500 sccm.

[0131] Example 3

[0132] This embodiment provides a short - circuit - proof electrochromic film structure, as Figure 1 shown. The short - circuit - proof electrochromic film structure includes a base layer 1, and a first transparent conductive layer 2, an insulating isolation layer 3, a cathode electrochromic layer 4, a dielectric layer 5, an ion - conducting layer 6, an anode electrochromic layer 7, and a second transparent conductive layer 8 are sequentially stacked above the base layer 1.

[0133] The insulating isolation layer 3 is made of titanium oxide, with a thickness of 25 nm and a refractive index of 2.5;

[0134] The base layer 1 is made of float glass, with a thickness of 0.4 mm;

[0135] The first transparent conductive layer 2 is an ITO film layer; with a thickness of 500 nm;

[0136] The cathode electrochromic layer 4 is made of tungsten oxide; with a thickness of 500 nm;

[0137] The dielectric layer 5 is a lithium layer; with a thickness of 300 nm;

[0138] The ion - conducting layer 6 is made of silicon oxide or silicon aluminum oxide; with a thickness of 25 nm;

[0139] The anode electrochromic layer 7 is made of tungsten nickel oxide; with a thickness of 500 nm;

[0140] The second transparent conductive layer 8 is an ITO film layer; with a thickness of 900 nm.

[0141] The preparation method of the short - circuit - proof electrochromic film structure includes:

[0142] Using the method of vacuum magnetron sputtering coating, the first transparent conductive layer, insulating isolation layer, cathode electrochromic layer, dielectric layer, ion - conducting layer, anode electrochromic layer, and second transparent conductive layer are sequentially coated above the base layer at a coating speed of 1 m / min;

[0143] Among them, during the coating process of the first transparent conductive layer, the power density of magnetron sputtering is 6 kw / m, the coating temperature is 230 °C, the coating pressure is 0.1 Pa, the oxygen flow rate is 1% of the total gas flow rate, and the argon flow rate is 500 sccm;

[0144] During the coating process of the insulating isolation layer, the power density of magnetron sputtering is 5 kw / m, the coating temperature is 400 °C, the coating pressure is 0.4 Pa; the gas includes oxygen and argon, the oxygen flow rate is 80% of the total gas flow rate, and the argon flow rate is 200 sccm;

[0145] During the deposition of the cathode electrochromic layer, the power density of magnetron sputtering is 10 kw / m, the coating temperature is 250 °C, the coating pressure is 4.0 Pa, the oxygen flow rate is 90% of the total gas flow rate, and the argon flow rate is 700 sccm;

[0146] During the deposition of the dielectric layer, the power density during magnetron sputtering is 10 kw / m, the coating temperature is 80 °C, the coating pressure is 1 Pa, and the argon flow rate is 700 sccm;

[0147] During the deposition of the ion conduction layer, the power density of magnetron sputtering is 12 kw / m, the coating temperature is 20 °C, the coating pressure is 0.1 Pa, the oxygen flow rate is 900% of the total gas flow rate, and the argon flow rate is 600 sccm;

[0148] During the deposition of the anode electrochromic layer, the power density of magnetron sputtering is 20 kw / m, the coating temperature is 20 °C, the coating pressure is 0.5 Pa, the oxygen flow rate is 90% of the total gas flow rate, and the argon flow rate is 800 sccm;

[0149] During the deposition of the second transparent conductive layer, the power density of magnetron sputtering is 4.8 kw / m, the coating temperature is 50 °C, the coating pressure is 0.7 Pa, the oxygen flow rate is 0.6% of the total gas flow rate, and the argon flow rate is 400 sccm.

[0150] Example 4

[0151] This example provides a short - circuit - proof electrochromic film structure. The difference between the short - circuit - proof electrochromic film structure and that of Example 1 is only that:

[0152] In this example, the thickness of the insulation isolation layer 3 is adjusted to 35 nm.

[0153] The preparation method of the short - circuit - proof electrochromic film structure is the same as that of Example 1.

[0154] Example 5

[0155] This example provides a short - circuit - proof electrochromic film structure. The difference between the short - circuit - proof electrochromic film structure and that of Example 1 is only that:

[0156] In this example, the thickness of the insulation isolation layer 3 is adjusted to 3 nm.

[0157] The preparation method of the short - circuit - proof electrochromic film structure is the same as that of Example 1.

[0158] Example 6

[0159] This example provides a short - circuit - proof electrochromic film structure. The difference between the short - circuit - proof electrochromic film structure and that of Example 1 is only that:

[0160] In this embodiment, during the deposition of the insulating isolation layer, the coating temperature of magnetron sputtering is adjusted to 200 °C.

[0161] The preparation method of the short - circuit - proof electrochromic film structure is the same as that of Embodiment 1.

[0162] Embodiment 7

[0163] This embodiment provides a short - circuit - proof electrochromic film structure. The difference between the short - circuit - proof electrochromic film structure and that of Embodiment 1 is only that:

[0164] In this embodiment, during the deposition of the insulating isolation layer, the coating temperature of magnetron sputtering is adjusted to 500 °C.

[0165] The preparation method of the short - circuit - proof electrochromic film structure is the same as that of Embodiment 1.

[0166] Embodiment 8

[0167] This embodiment provides a short - circuit - proof electrochromic film structure. The difference between the short - circuit - proof electrochromic film structure and that of Embodiment 1 is only that:

[0168] In this embodiment, during the deposition of the insulating isolation layer, the power density of magnetron sputtering is adjusted to 2 kw / m.

[0169] The preparation method of the short - circuit - proof electrochromic film structure is the same as that of Embodiment 1.

[0170] Embodiment 9

[0171] This embodiment provides a short - circuit - proof electrochromic film structure. The difference between the short - circuit - proof electrochromic film structure and that of Embodiment 1 is only that:

[0172] In this embodiment, during the deposition of the insulating isolation layer, the power density of magnetron sputtering is adjusted to 20 kw / m.

[0173] The preparation method of the short - circuit - proof electrochromic film structure is the same as that of Embodiment 1.

[0174] Embodiment 10

[0175] This embodiment provides a short - circuit - proof electrochromic film structure. The difference between the short - circuit - proof electrochromic film structure and that of Embodiment 1 is only that:

[0176] In this embodiment, the material of the insulating isolation layer is adjusted to tungsten oxide.

[0177] The preparation method of the short - circuit - proof electrochromic film structure is the same as that of Embodiment 1.

[0178] Comparative Example 1

[0179] This comparative example provides a short - circuit - proof electrochromic film structure. The difference between the short - circuit - proof electrochromic film structure and that of Example 1 is only that:

[0180] This comparative example omits the setting of the insulating isolation layer.

[0181] The preparation method of the short - circuit - proof electrochromic film structure is the same as that of Example 1.

[0182] Comparative Example 2

[0183] This comparative example provides a short - circuit - proof electrochromic film structure. The difference between the short - circuit - proof electrochromic film structure and that of Example 1 is only that:

[0184] This comparative example adjusts the setting position of the insulating isolation layer to between the anodic electrochromic layer and the second transparent conductive layer.

[0185] The preparation method of the short - circuit - proof electrochromic film structure is the same as that of Example 1.

[0186] Comparative Example 3

[0187] This comparative example provides a short - circuit - proof electrochromic film structure. The difference between the short - circuit - proof electrochromic film structure and that of Example 1 is only that:

[0188] This comparative example adjusts the setting position of the insulating isolation layer to between the anodic electrochromic layer and the second transparent conductive layer, and adjusts the material of the insulating isolation layer to nickel tungsten oxide.

[0189] The preparation method of the short - circuit - proof electrochromic film structure is the same as that of Example 1,

[0190] Performance detection:

[0191] Perform leakage current testing and coloring time testing on the short - circuit - proof electrochromic film structures provided in the above - mentioned examples and comparative examples when a voltage of 3V is applied. The results are shown in Table 1.

[0192] Among them, the electrochromic product includes:

[0193] Table 1

[0194]

[0195]

[0196] It can be seen from Table 1 that:

[0197] (1) Through comprehensive analysis of Examples 1 - 3, it can be known that the present invention significantly improves the leakage current caused by short - circuit of the electrochromic film layer by setting an insulating isolation layer between the first transparent conductive layer and the cathodic electrochromic layer, and at the same time can meet the requirement of coloring time;

[0198] (2) By comprehensively analyzing Examples 1 and 4 - 5, it can be seen that if the thickness of the insulation isolation layer is too thick, the coloring speed will become slow, and if it is too thin, the leakage current will become large and the coloring speed will become slow.

[0199] (3) By comprehensively analyzing Examples 1 and 6 - 9, it can be seen that the process parameters during the plating process of the insulation isolation layer will affect the working effect of the insulation isolation layer.

[0200] More specifically, when the coating temperature during the plating process is too high, it will cause fragmentation (such as in Example 7), and if it is too low, the crystallinity of the film layer will be poor and the leakage current will become large.

[0201] When the magnetron sputtering power density during the plating process is too high, it will cause insufficient oxidation, poor insulation, and an increase in leakage current. If it is too low, the coating energy will be low, the compactness of the film layer will be poor, and the leakage current will increase.

[0202] (4) By comprehensively analyzing Examples 1, 10 and Comparative Examples 1 - 3, it can be seen that the setting position and material of the insulation isolation layer will both affect the coloring time or leakage current of the electrochromic product.

[0203] If the material of the insulation isolation layer is adjusted to tungsten oxide, it will have no effect, the leakage current will increase, and the coloring time will become longer.

[0204] If the setting of the insulation isolation layer is omitted, the leakage current will increase and the coloring time will become longer.

[0205] If the insulation isolation layer is adjusted between the anode electrochromic layer and the second transparent conductive layer, the leakage current will be large and the coloring time will be long.

[0206] If the insulation isolation layer is adjusted between the anode electrochromic layer and the second transparent conductive layer and the material of the insulation isolation layer is adjusted to nickel tungsten oxide, the leakage current will be large and the coloring time will be long.

[0207] In summary, by optimizing the film layer structure of the electrochromic product of the present invention, the improvement of the leakage current caused by short - circuit of the electrochromic film layer is realized, and at the same time, the requirement of the coloring time is further ensured.

[0208] The applicant declares that the above - mentioned is only the specific implementation manner 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 within the technical scope disclosed by the present invention by those skilled in the art all fall within the protection scope and the disclosure scope of the present invention.

Claims

1. An anti-short-circuit electrochromic film structure, characterized in that, The short-circuit-proof electrochromic film structure includes a base layer, and a first transparent conductive layer, an insulating isolation layer, a cathode electrochromic layer, a dielectric layer, an ion conduction layer, an anode electrochromic layer, and a second transparent conductive layer are sequentially stacked above the base layer.

2. The anti-short circuit electrochromic film structure according to claim 1, characterized in that The material of the insulating isolation layer includes titanium oxide or; Preferably, the thickness of the insulating isolation layer is 5-30 nm; Preferably, the refractive index of the insulating isolation layer is 2.3-2.

5.

3. The short-circuit-proof electrochromic film structure according to claim 1 or 2, characterized in that The material of the base layer includes float glass; Preferably, the thickness of the base layer is 0.4-5.0 mm.

4. The short-circuit-proof electrochromic film structure according to any one of claims 1-3, characterized in that The first transparent conductive layer includes an ITO film layer; Preferably, the material of the cathode electrochromic layer includes tungsten oxide; Preferably, the dielectric layer includes a lithium layer; Preferably, the material of the ion conduction layer includes silicon oxide or silicon aluminum oxide; Preferably, the material of the anode electrochromic layer includes tungsten nickel oxide; Preferably, the second transparent conductive layer includes an ITO film layer.

5. The short-circuit-proof electrochromic film structure according to any one of claims 1-4, characterized in that, The thickness of the first transparent conductive layer is 100-500 nm; Preferably, the thickness of the cathode electrochromic layer is 200-500 nm; Preferably, the thickness of the dielectric layer is 100-300 nm; Preferably, the thickness of the ion conduction layer is 5-25 nm; Preferably, the thickness of the anode electrochromic layer is 200-500 nm; Preferably, the thickness of the second transparent conductive layer is 300-900 nm.

6. A preparation method of the short-circuit-proof electrochromic film structure according to any one of claims 1-5, characterized in that, The preparation method includes: Using the method of vacuum magnetron sputtering coating, the first transparent conductive layer, the insulating isolation layer, the cathode electrochromic layer, the dielectric layer, the ion conduction layer, the anode electrochromic layer, and the second transparent conductive layer are sequentially coated above the base layer.

7. The preparation method according to claim 6, characterized in that, The coating speed during the coating process is 0.1-1 m / min.

8. The preparation method according to claim 6 or 7, characterized in that, During the process of coating the insulating isolation layer, the power density of magnetron sputtering is 5-15 kw / m.

9. The preparation method according to any one of claims 6-8, characterized in that, During the process of coating the insulating isolation layer, the coating temperature of magnetron sputtering is 250-400 °C; Preferably, during the process of coating the insulating isolation layer, the coating pressure of magnetron sputtering is 0.1-1 Pa.

10. The preparation method according to any one of claims 6-9, characterized in that, During the process of coating the insulating isolation layer, the gases for magnetron sputtering include oxygen and argon; Preferably, the flow rate of oxygen is 20-80% of the total gas flow rate; Preferably, the flow rate of argon is 100-1000 sccm.

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