Electrochromic device, preparation method and electrochromic product

Abstract

The invention relates to an electrochromic device, a preparation method and an electrochromic product, in particular to the field of electrochromism, and aims to overcome the defect that when an electrochromic film fades into a transparent state, the color of the device is slightly yellow. Comprising a first conductive layer, an isolation layer, a cathode electrochromic layer, an ion conduction layer, an anode electrochromic layer, an IA group element layer and a second conductive layer which are sequentially arranged on a substrate, the anode electrochromic layer comprises tungsten nickel oxide X oxide, and X comprises one or a combination of at least two of tantalum, titanium or molybdenum. According to the electrochromic device provided by the invention, components in the electrochromic device, especially the anode electrochromic layer, are optimized, so that the electrochromic device can achieve a transparent effect during color fading, and the problem of yellowing does not occur.

Description

Technical Field

[0001] The present invention relates to the field of electrochromism, and in particular to an electrochromic device, a preparation method, and an electrochromic product. Background Art

[0002] At present, as the application scope of electrochromic products becomes increasingly wide, vehicle rearview mirrors, sunroofs, military camouflage functions, and windows in buildings can all use electrochromic technology to achieve different purposes.

[0003] For example, CN113267931A discloses an electrochromic film, which includes a base layer, a first transparent conductive ion layer located on the base layer, an electrochromic layer located on the transparent conductive ion layer, and a second transparent conductive ion layer located on the electrochromic layer. Electrodes are connected to the edges of the first transparent conductive ion layer and the second transparent conductive ion layer, and the electrochromic layer contains an electrochromic polymer and conductive ions.

[0004] CN108061982A discloses an electrochromic glass comprising two sheets of glass with indium tin oxide (ITO) electrodes formed on their surfaces. The ITO electrodes face each other with a filler region between them. The edges are glued together with a filler adhesive. Bistable liquid crystals are poured into the filler region. The bistable liquid crystals twist under voltage. When a voltage is applied to the electrodes, the liquid crystals twist, switching between transparent and opaque, changing their transmittance and transparency. Once the state is triggered, the power can be turned off, and the liquid crystals will remain in the specific twisted state, saving energy.

[0005] However, although the existing film layer structure can achieve electrochromism, the device color tends to be yellowish when it fades to a transparent state. Existing technologies have reduced the yellowing of the device by thinning the tungsten oxide in the cathode electrochromic layer, the nickel oxide in the anode electrochromic layer, or the tungsten oxide nickel layer. However, this not only fails to completely solve the problem of the yellowing of the device, but also brings the risk of not having a deep color due to the thinning of the film thickness.

[0006] In summary, the current electrochromic film still has the defect that the device color is yellowish when it fades to a transparent state. Summary of the Invention

[0007] In view of the problems existing in the prior art, the purpose of the present invention is to provide an electrochromic device, a preparation method, and an electrochromic product to solve the defect that the electrochromic film still has a yellowish color when the device fades to a transparent state.

[0008] To achieve this object, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides an electrochromic device, comprising: a first conductive layer, an insulating layer, a cathode electrochromic layer, an ion conducting layer, an anode electrochromic layer, a Group IA element layer, and a second conductive layer sequentially disposed on a substrate;

[0010] The anode electrochromic layer includes tungsten nickel oxide X oxide, where X includes one or a combination of at least two of tantalum, titanium or molybdenum.

[0011] The electrochromic device provided by the present invention optimizes the components in the electrochromic device, especially the anode electrochromic layer, so that the electrochromic device can achieve a transparent effect when fading without the problem of yellowing.

[0012] As a preferred technical solution of the present invention, the substrate comprises: glass with a thickness of 0.4-5 mm.

[0013] Preferably, the first conductive layer includes: an ITO film layer and / or a FTO film layer.

[0014] Preferably, the thickness of the first conductive layer is 100-900 nm.

[0015] As a preferred technical solution of the present invention, the insulating layer includes a titanium oxide layer.

[0016] Preferably, the thickness of the insulating layer is 25-100 nm.

[0017] As a preferred technical solution of the present invention, the cathode electrochromic layer includes: a tungsten oxide layer.

[0018] Preferably, the cathode electrochromic layer has a thickness of 200-500 nm.

[0019] As a preferred technical solution of the present invention, the ion conducting layer includes: one of a tungsten oxide layer, a silicon oxide layer, a silicon aluminum oxide layer or a tungsten nickel oxide layer.

[0020] Preferably, the thickness of the ion conducting layer is 25-100 nm.

[0021] As a preferred technical solution of the present invention, the target material used in the preparation of the anode electrochromic layer comprises, by mass percentage, 35-45% tungsten, 35-45% nickel, and the balance is X.

[0022] Preferably, the thickness of the anode electrochromic layer is 200-500 nm.

[0023] Preferably, the Group IA element layer includes one of a lithium layer, a sodium layer or a potassium layer.

[0024] Preferably, the thickness of the Group IA element layer is 50-150 nm.

[0025] As a preferred technical solution of the present invention, the second conductive layer includes: an ITO film layer.

[0026] Preferably, the thickness of the second conductive layer is 200-900 nm.

[0027] In a second aspect, the present invention provides a method for preparing an electrochromic device, the preparation method comprising: sequentially growing a first conductive layer, an insulating layer, a cathode electrochromic layer, an ion conducting layer, an anode electrochromic layer, a Group IA element layer, and a second conductive layer on a substrate.

[0028] As a preferred technical solution of the present invention, the thickness of the conductive layer obtained by growing the first conductive layer is 100-900 nm.

[0029] Preferably, the first conductive layer is grown by physical magnetron sputtering.

[0030] Preferably, the power density of the growth of the first conductive layer is 2-5 kW / m.

[0031] Preferably, the coating temperature for growing the first conductive layer is 250-350°C.

[0032] Preferably, the coating pressure for growing the first conductive layer is 0.1-0.8 Pa.

[0033] Preferably, the flow rate of argon gas during the growth of the first conductive layer is 200-800 sccm.

[0034] Preferably, the flow rate of oxygen during the growth of the first conductive layer is 0.1-0.6% of the total process gas flow.

[0035] Preferably, the coating speed of the first conductive layer is 0.1-1 m / min.

[0036] Preferably, the thickness of the insulating layer obtained by growing the insulating layer is 25-100 nm.

[0037] Preferably, the insulating layer is grown by physical magnetron sputtering coating.

[0038] Preferably, the power density of the insulating layer growth is 5-15 kW / m.

[0039] Preferably, the coating temperature for growing the insulating layer is 250-350°C.

[0040] Preferably, the coating pressure for growing the insulating layer is 0.3-0.8 Pa.

[0041] Preferably, the flow rate of argon gas during the growth of the isolation layer is 50-1000 sccm.

[0042] Preferably, the flow rate of oxygen during the growth of the insulation layer is 30-80% of the total process gas flow.

[0043] Preferably, the coating speed of the insulating layer growth is 0.1-1 m / min.

[0044] Preferably, the thickness of the conductive layer obtained by growing the cathode electrochromic layer is 200-500 nm.

[0045] Preferably, the cathode electrochromic layer is grown by physical magnetron sputtering coating.

[0046] Preferably, the power density of the cathode electrochromic layer growth is 10-20 kW / m.

[0047] Preferably, the coating temperature for growing the cathode electrochromic layer is 250-380°C.

[0048] Preferably, the coating pressure for growing the cathode electrochromic layer is 0.5-4 Pa.

[0049] Preferably, the flow rate of argon gas during the growth of the cathode electrochromic layer is ≤1000 sccm.

[0050] Preferably, the flow rate of oxygen during the growth of the cathode electrochromic layer is 50-100% of the total process gas flow.

[0051] Preferably, the coating speed of the cathode electrochromic layer is 0.1-1 m / min.

[0052] Preferably, the thickness of the ion conducting layer obtained by growing the ion conducting layer is 25-100 nm.

[0053] Preferably, the ion conducting layer is grown by physical magnetron sputtering coating.

[0054] Preferably, the power density of the ion conducting layer growth is 5-10 kW / m.

[0055] Preferably, the coating temperature for growing the ion conducting layer is 30-80°C.

[0056] Preferably, the coating pressure for growing the ion conductive layer is 0.5-4Pa.

[0057] Preferably, the flow rate of argon gas during the growth of the ion conducting layer is ≤500 sccm.

[0058] Preferably, the flow rate of oxygen during the growth of the ion conducting layer is 65-100% of the total process gas flow.

[0059] Preferably, the coating speed of the ion conductive layer is 0.1-1 m / min.

[0060] Preferably, the thickness of the conductive layer obtained by growing the anode electrochromic layer is 200-500 nm.

[0061] Preferably, the anode electrochromic layer is grown by physical magnetron sputtering coating.

[0062] Preferably, the power density of the growth of the anode electrochromic layer is 10-20 kW / m.

[0063] Preferably, the coating temperature for growing the anode electrochromic layer is 30-100°C.

[0064] Preferably, the coating pressure for growing the anode electrochromic layer is 0.5-4 Pa.

[0065] Preferably, the flow rate of argon gas during the growth of the anode electrochromic layer is ≤500 sccm.

[0066] Preferably, the flow rate of oxygen during the growth of the anode electrochromic layer is 60-100% of the total process gas flow.

[0067] Preferably, the coating speed of the anode electrochromic layer is 0.1-1 m / min.

[0068] Preferably, the thickness of the conductive layer obtained by growing the Group IA element layer is 50-150 nm.

[0069] Preferably, the method of growing the group IA element layer includes: physical magnetron sputtering coating.

[0070] Preferably, the power density for growing the group IA element layer is 2-10 kW / m.

[0071] Preferably, the coating temperature for growing the group IA element layer is 30-80°C.

[0072] Preferably, the coating pressure for growing the group IA element layer is 0.1-1 Pa.

[0073] Preferably, the flow rate of argon gas during the growth of the Group IA element layer is 100-1000 sccm.

[0074] Preferably, the coating speed of the IA group element layer is 0.1-1 m / min.

[0075] Preferably, the thickness of the conductive layer obtained by growing the second conductive layer is 200-900 nm.

[0076] Preferably, the second conductive layer is grown by physical magnetron sputtering.

[0077] Preferably, the power density of the second conductive layer during growth is 2-6 kW / m.

[0078] Preferably, the coating temperature for growing the second conductive layer is 50-150°C.

[0079] Preferably, the coating pressure for growing the second conductive layer is 0.1-1 Pa.

[0080] Preferably, the flow rate of argon gas during the growth of the second conductive layer is 100-500 sccm.

[0081] Preferably, the flow rate of oxygen during the growth of the second conductive layer is 0.1-1% of the total process gas flow.

[0082] Preferably, the coating speed of the second conductive layer is 0.1-1 m / min.

[0083] In a third aspect, the present invention provides an electrochromic product, comprising the electrochromic layer described in the first aspect.

[0084] Compared with the existing technical solutions, the present invention has the following beneficial effects:

[0085] The electrochromic device provided by the present invention achieves a good electrochromic effect by specifically designing the anode electrochromic layer and selecting tungsten nickel tantalum, titanium or molybdenum as the anode electrochromic layer to cooperate with the cathode electrochromic layer. It can fade to a transparent state without affecting the coloring depth, that is, it can ensure that the device does not turn yellow after fading, ensuring that the electrochromic product has a good sensory experience effect. The b value of the obtained electrochromic device is ≤+7 and >0. BRIEF DESCRIPTION OF THE DRAWINGS

[0086] Figure 1 is a schematic structural diagram of an electrochromic device provided by an embodiment of the present invention;

[0087] Figure 2 This is a photograph of the electrochromic device obtained in Example 1 of the present invention in a faded state;

[0088] Figure 3 This is a photograph of the electrochromic device obtained in Comparative Example 1 of the present invention in a faded state.

[0089] In the figure: 100 - substrate, 200 - first conductive layer, 300 - insulating layer, 400 - cathode electrochromic layer, 500 - ion conducting layer, 600 - anode electrochromic layer, 700 - IA group element layer, 800 - second conductive layer.

[0090] The present invention is further described in detail below. However, the following examples are merely 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. DETAILED DESCRIPTION

[0091] To better illustrate the present invention and facilitate understanding of the technical solutions of the present invention, typical but non-limiting embodiments of the present invention are as follows:

[0092] 1. This embodiment provides an electrochromic device, which includes: a first conductive layer 200, an insulating layer 300, a cathode electrochromic layer 400, an ion conducting layer 500, an anode electrochromic layer 600, an IA group element layer 700, and a second conductive layer 800, which are sequentially arranged on a substrate 100, and the structure is as follows: Figure 1 shown.

[0093] The substrate 100 includes: glass with a thickness of 0.4-5 mm, for example, it can be 0.4 mm, 0.6 mm, 0.8 mm, 1 mm, 1.5 mm, 2 mm, 2.5 mm, 3 mm, 3.5 mm, 4 mm, 4.5 mm or 5 mm, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0094] Wherein, the first conductive layer 200 includes: an ITO film layer and / or a FTO film layer.

[0095] The thickness of the first conductive layer 200 is 100-900 nm, for example, 100 nm, 200 nm, 300 nm, 400 nm, 500 nm, 600 nm, 700 nm, 800 nm or 900 nm, but is not limited to the listed values. Other values ​​not listed within the range also meet the requirements.

[0096] Wherein, the isolation layer 300 includes a titanium oxide layer.

[0097] The thickness of the insulating layer 300 is 25-100 nm, for example, it can be 25 nm, 30 nm, 35 nm, 40 nm, 45 nm, 50 nm, 55 nm, 60 nm, 65 nm, 70 nm, 75 nm, 80 nm, 85 nm, 90 nm, 95 nm or 100 nm, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0098] Wherein, the cathode electrochromic layer 400 includes: a tungsten oxide layer.

[0099] The thickness of the cathode electrochromic layer 400 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. Other values ​​not listed within this range also meet the requirements.

[0100] The ion conducting layer 500 includes one of a tungsten oxide layer, a silicon oxide layer, a silicon aluminum oxide layer or a tungsten nickel oxide layer.

[0101] The thickness of the ion conducting layer 500 is 25-100 nm, for example, 25 nm, 30 nm, 35 nm, 40 nm, 45 nm, 50 nm, 55 nm, 60 nm, 65 nm, 70 nm, 75 nm, 80 nm, 85 nm, 90 nm, 95 nm or 100 nm, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0102] The anode electrochromic layer 600 includes tungsten nickel oxide X oxide, where X includes one or a combination of at least two of tantalum, titanium or molybdenum.

[0103] Among them, the target material used in the preparation of the anode electrochromic layer 600 includes, by mass percentage, 35-45% tungsten, 35-45% nickel, and the balance is X. The tungsten content can be, for example, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44% or 45%, and the nickel content can be, for example, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44% or 45%, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0104] The thickness of the anode electrochromic layer 600 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. Other values ​​not listed within this range also meet the requirements.

[0105] The group IA element layer 700 includes a lithium layer, a sodium layer or a potassium layer.

[0106] Among them, the thickness of the IA group element layer 700 is 50-150nm, for example, it can be 50nm, 60nm, 70nm, 80nm, 90nm, 100nm, 110nm, 120nm, 130nm, 140nm or 150nm, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0107] Wherein, the second conductive layer 800 includes: an ITO film layer.

[0108] Among them, the thickness of the second conductive layer 800 is 200-900nm, for example, it can be 200nm, 250nm, 300nm, 350nm, 400nm, 450nm, 500nm, 550nm, 600nm, 650nm, 700nm, 750nm, 800nm, 850nm or 900nm, but is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0109] In the present invention, omitting the insulating layer 300 or replacing the titanium oxide layer with a silicon oxide layer can cause a short circuit between the upper and lower conductive layers of the resulting electrochromic device, resulting in cosmetic defects and the inability to achieve full-surface color change. Furthermore, omitting the Group IA element layer 700 or replacing it with another material layer, such as Ag, can prevent the electrochromic device from changing color due to the lack of ion transfer.

[0110] 2. This embodiment provides a method for preparing an electrochromic device, which includes: sequentially growing a first conductive layer, an insulating layer, a cathode electrochromic layer, an ion conducting layer, an anode electrochromic layer, a Group IA element layer, and a second conductive layer on a substrate 100.

[0111] The electrochromic device includes: a first conductive layer 200, an insulating layer 300, a cathode electrochromic layer 400, an ion conducting layer 500, an anode electrochromic layer 600, a group IA element layer 700 and a second conductive layer 800 arranged in sequence on a substrate 100.

[0112] The substrate 100 includes: glass with a thickness of 0.4-5 mm, for example, it can be 0.4 mm, 0.6 mm, 0.8 mm, 1 mm, 1.5 mm, 2 mm, 2.5 mm, 3 mm, 3.5 mm, 4 mm, 4.5 mm or 5 mm, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0113] Wherein, the first conductive layer 200 includes: an ITO film layer and / or a FTO film layer.

[0114] The thickness of the first conductive layer 200 is 100-900 nm, for example, 100 nm, 200 nm, 300 nm, 400 nm, 500 nm, 600 nm, 700 nm, 800 nm or 900 nm, but is not limited to the listed values. Other values ​​not listed within the range also meet the requirements.

[0115] Wherein, the isolation layer 300 includes a titanium oxide layer.

[0116] The thickness of the insulating layer 300 is 25-100 nm, for example, it can be 25 nm, 30 nm, 35 nm, 40 nm, 45 nm, 50 nm, 55 nm, 60 nm, 65 nm, 70 nm, 75 nm, 80 nm, 85 nm, 90 nm, 95 nm or 100 nm, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0117] Wherein, the cathode electrochromic layer 400 includes: a tungsten oxide layer.

[0118] The thickness of the cathode electrochromic layer 400 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. Other values ​​not listed within this range also meet the requirements.

[0119] The ion conducting layer 500 includes one of a tungsten oxide layer, a silicon oxide layer, a silicon aluminum oxide layer or a tungsten nickel oxide layer.

[0120] The thickness of the ion conducting layer 500 is 25-100 nm, for example, 25 nm, 30 nm, 35 nm, 40 nm, 45 nm, 50 nm, 55 nm, 60 nm, 65 nm, 70 nm, 75 nm, 80 nm, 85 nm, 90 nm, 95 nm or 100 nm, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0121] The anode electrochromic layer 600 includes tungsten nickel oxide X oxide, where X includes one or a combination of at least two of tantalum, titanium or molybdenum.

[0122] Among them, the target material used in the preparation of the anode electrochromic layer 600 includes, by mass percentage, 35-45% tungsten, 35-45% nickel, and the balance is X. The tungsten content can be, for example, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44% or 45%, and the nickel content can be, for example, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44% or 45%, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0123] The thickness of the anode electrochromic layer 600 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. Other values ​​not listed within this range also meet the requirements.

[0124] The group IA element layer 700 includes a lithium layer, a sodium layer or a potassium layer.

[0125] Among them, the thickness of the IA group element layer 700 is 50-150nm, for example, it can be 50nm, 60nm, 70nm, 80nm, 90nm, 100nm, 110nm, 120nm, 130nm, 140nm or 150nm, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0126] Wherein, the second conductive layer 800 includes: an ITO film layer.

[0127] Among them, the thickness of the second conductive layer 800 is 200-900nm, for example, it can be 200nm, 250nm, 300nm, 350nm, 400nm, 450nm, 500nm, 550nm, 600nm, 650nm, 700nm, 750nm, 800nm, 850nm or 900nm, but is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0128] The thickness of the conductive layer obtained by growing the first conductive layer is 100-900 nm, for example, it can be 100 nm, 200 nm, 300 nm, 400 nm, 500 nm, 600 nm, 700 nm, 800 nm or 900 nm, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0129] Wherein, the first conductive layer is grown in a manner including physical magnetron sputtering coating.

[0130] Among them, the power density of the growth of the first conductive layer is 2-5kW / m, for example, it can be 2kW / m, 2.5kW / m, 3kW / m, 3.5kW / m, 4kW / m, 4.5kW / m or 5kW / m, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0131] Among them, the coating temperature for growing the first conductive layer is 250-350°C, for example, it can be 250°C, 260°C, 270°C, 280°C, 290°C, 300°C, 310°C, 320°C, 330°C, 340°C or 350°C, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0132] Among them, the coating pressure for the growth of the first conductive layer is 0.1-0.8Pa, for example, it can be 0.1Pa, 0.2Pa, 0.3Pa, 0.4Pa, 0.5Pa, 0.6Pa, 0.7Pa or 0.8Pa, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0133] Among them, the flow rate of argon gas in the growth of the first conductive layer is 200-800sccm, for example, it can be 200sccm, 250sccm, 300sccm, 350sccm, 400sccm, 450sccm, 500sccm, 550sccm, 600sccm, 650sccm, 700sccm, 750sccm or 800sccm, etc., but is not limited to the listed values, and other unlisted values ​​within this range also meet the requirements.

[0134] Among them, the flow rate of oxygen in the growth of the first conductive layer is 0.1-0.6% of the total process gas flow, for example, it can be 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, 0.55% or 0.6%, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0135] Among them, the coating speed of the growth of the first conductive layer is 0.1-1m / min, for example, it can be 0.1m / min, 0.1m / min, 0.2m / min, 0.3m / min, 0.4m / min, 0.5m / min, 0.6m / min, 0.7m / min, 0.8m / min, 0.9m / min or 1m / min, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0136] The thickness of the insulating layer obtained by growing the insulating layer is 25-100 nm, for example, it can be 25 nm, 30 nm, 35 nm, 40 nm, 45 nm, 50 nm, 55 nm, 60 nm, 65 nm, 70 nm, 75 nm, 80 nm, 85 nm, 90 nm, 95 nm or 100 nm, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0137] Wherein, the method of growing the isolation layer includes: physical magnetron sputtering coating.

[0138] Among them, the power density of the growth of the insulating layer is 5-15kW / m, for example, it can be 5kW / m, 6kW / m, 7kW / m, 8kW / m, 9kW / m, 10kW / m, 11kW / m, 12kW / m, 13kW / m, 14kW / m or 15kW / m, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0139] Among them, the coating temperature for the growth of the insulating layer is 250-350℃, for example, it can be 250℃, 260℃, 270℃, 280℃, 290℃, 300℃, 310℃, 320℃, 330℃, 340℃ or 350℃, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0140] Among them, the coating pressure for the growth of the insulating layer is 0.3-0.8Pa, for example, it can be 0.3Pa, 0.35Pa, 0.4Pa, 0.45Pa, 0.5Pa, 0.55Pa, 0.6Pa, 0.65Pa, 0.7Pa, 0.75Pa or 0.8Pa, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0141] Among them, the flow rate of argon gas in the growth of the isolation layer is 50-1000sccm, for example, it can be 50sccm, 60sccm, 70sccm, 80sccm, 90sccm, 100sccm, 200sccm, 300sccm, 400sccm, 500sccm, 600sccm, 700sccm, 800sccm, 900sccm or 1000sccm, etc., but is not limited to the listed values, and other unlisted values ​​within this range also meet the requirements.

[0142] Among them, the flow rate of oxygen in the growth of the insulating layer is 30-80% of the total process gas flow, for example, it can be 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75% or 80%, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0143] Among them, the coating speed of the insulating layer growth is 0.1-1m / min, for example, it can be 0.1m / min, 0.1m / min, 0.2m / min, 0.3m / min, 0.4m / min, 0.5m / min, 0.6m / min, 0.7m / min, 0.8m / min, 0.9m / min or 1m / min, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0144] The thickness of the conductive layer grown from 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. Other values ​​not listed within this range also meet the requirements.

[0145] Wherein, the cathode electrochromic layer is grown in a manner including physical magnetron sputtering coating.

[0146] Among them, the power density of the growth of the cathode electrochromic layer is 10-20kW / m, for example, it can be 10kW / m, 11kW / m, 12kW / m, 13kW / m, 14kW / m, 15kW / m, 16kW / m, 17kW / m, 18kW / m, 19kW / m or 20kW / m, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0147] Among them, the coating temperature for growing the cathode electrochromic layer is 250-380°C, for example, it can be 250°C, 260°C, 270°C, 280°C, 290°C, 300°C, 310°C, 320°C, 330°C, 340°C, 350°C, 360°C, 370°C or 380°C, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0148] Among them, the coating pressure for the growth of the cathode electrochromic layer is 0.5-4Pa, for example, it can be 0.5Pa, 0.6Pa, 0.7Pa, 0.8Pa, 0.9Pa, 1Pa, 1.5Pa, 2Pa, 2.5Pa, 3Pa, 3.5Pa or 4Pa, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0149] Among them, the flow rate of argon gas in the growth of the cathode electrochromic layer is ≤1000sccm, for example, it can be 1000sccm, 900sccm, 800sccm, 700sccm, 600sccm, 500sccm, 400sccm, 300sccm, 200sccm, 100sccm, 50sccm, 10sccm, 5sccm, 1sccm or 0sccm, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0150] Among them, the flow rate of oxygen in the growth of the cathode electrochromic layer is 50-100% of the total process gas flow, for example, it can be 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95% or 100%, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0151] Among them, the coating speed of the cathode electrochromic layer growth is 0.1-1m / min, for example, it can be 0.1m / min, 0.1m / min, 0.2m / min, 0.3m / min, 0.4m / min, 0.5m / min, 0.6m / min, 0.7m / min, 0.8m / min, 0.9m / min or 1m / min, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0152] The thickness of the ion conducting layer obtained by growing the ion conducting layer is 25-100 nm, for example, it can be 25 nm, 30 nm, 35 nm, 40 nm, 45 nm, 50 nm, 55 nm, 60 nm, 65 nm, 70 nm, 75 nm, 80 nm, 85 nm, 90 nm, 95 nm or 100 nm, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0153] Wherein, the method of growing the ion conducting layer includes: physical magnetron sputtering coating.

[0154] Among them, the power density of the growth of the ion conductive layer is 5-10kW / m, for example, it can be 5kW / m, 5.5kW / m, 6kW / m, 6.5kW / m, 7kW / m, 7.5kW / m, 8kW / m, 8.5kW / m, 9kW / m, 9.5kW / m or 10kW / m, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0155] Among them, the coating temperature for the growth of the ion conductive layer is 30-80°C, for example, it can be 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, 75°C or 80°C, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0156] Among them, the coating pressure for the growth of the ion conductive layer is 0.5-4Pa, for example, it can be 0.5Pa, 1Pa, 1.5Pa, 2Pa, 2.5Pa, 3Pa, 3.5Pa or 4Pa, but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0157] Among them, the flow rate of argon gas in the growth of the ion conductive layer is ≤500sccm, for example, it can be 500sccm, 400sccm, 300sccm, 200sccm, 100sccm, 50sccm, 10sccm, 5sccm, 1sccm or 0sccm, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0158] Among them, the flow rate of oxygen in the growth of the ion conductive layer is 65-100% of the total process gas flow, for example, it can be 65%, 70%, 75%, 80%, 85%, 90%, 95% or 100%, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0159] Among them, the coating speed of the growth of the ion conductive layer is 0.1-1m / min, for example, it can be 0.1m / min, 0.1m / min, 0.2m / min, 0.3m / min, 0.4m / min, 0.5m / min, 0.6m / min, 0.7m / min, 0.8m / min, 0.9m / min or 1m / min, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0160] The thickness of the conductive layer obtained by growing the anode electrochromic layer is 200-500 nm, for example, it can be 200 nm, 220 nm, 240 nm, 260 nm, 280 nm, 300 nm, 320 nm, 340 nm, 360 nm, 380 nm, 400 nm, 420 nm, 440 nm, 460 nm, 480 nm or 500 nm, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0161] Wherein, the growth method of the anode electrochromic layer includes: physical magnetron sputtering coating.

[0162] Among them, the power density of the growth of the anode electrochromic layer is 10-20kW / m, for example, it can be 10kW / m, 11kW / m, 12kW / m, 13kW / m, 14kW / m, 15kW / m, 16kW / m, 17kW / m, 18kW / m, 19kW / m or 20kW / m, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0163] Among them, the coating temperature for growing the anode electrochromic layer is 30-100°C, for example, it can be 30°C, 40°C, 50°C, 60°C, 70°C, 80°C, 90°C or 100°C, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0164] Among them, the coating pressure for the growth of the anode electrochromic layer is 0.5-4Pa, for example, it can be 0.5Pa, 0.6Pa, 0.7Pa, 0.8Pa, 0.9Pa, 1Pa, 1.5Pa, 2Pa, 2.5Pa, 3Pa, 3.5Pa or 4Pa, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0165] Among them, the flow rate of argon gas in the growth of the anode electrochromic layer is ≤500sccm, for example, it can be 500sccm, 400sccm, 300sccm, 200sccm, 100sccm, 50sccm, 10sccm, 5sccm, 1sccm or 0sccm, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0166] Among them, the flow rate of oxygen in the growth of the anode electrochromic layer is 60-100% of the total process gas flow, for example, it can be 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95% or 100%, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0167] Among them, the coating speed of the growth of the anode electrochromic layer is 0.1-1m / min, for example, it can be 0.1m / min, 0.1m / min, 0.2m / min, 0.3m / min, 0.4m / min, 0.5m / min, 0.6m / min, 0.7m / min, 0.8m / min, 0.9m / min or 1m / min, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0168] Among them, the thickness of the conductive layer obtained by growing the IA group element layer is 50-150nm, for example, it can be 50nm, 60nm, 70nm, 80nm, 90nm, 100nm, 110nm, 120nm, 130nm, 140nm or 150nm, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0169] Wherein, the method of growing the group IA element layer includes: physical magnetron sputtering coating.

[0170] Among them, the power density of the growth of the IA group element layer is 2-10kW / m, for example, it can be 2kW / m, 2.5kW / m, 3kW / m, 3.5kW / m, 4kW / m, 4.5kW / m, 5kW / m, 5.5kW / m, 6kW / m, 6.5kW / m, 7kW / m, 7.5kW / m, 8kW / m, 8.5kW / m, 9kW / m, 9.5kW / m or 10kW / m, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0171] Among them, the coating temperature for growing the IA group element layer is 30-80°C, for example, it can be 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, 60°C, 65°C, 70°C, 75°C or 80°C, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0172] Among them, the coating pressure for growing the IA group element layer is 0.1-1Pa, for example, it can be 0.1Pa, 0.2Pa, 0.3Pa, 0.4Pa, 0.5Pa, 0.6Pa, 0.7Pa, 0.8Pa, 0.9Pa or 1Pa, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0173] Among them, the flow rate of argon gas in the growth of the IA group element layer is 100-1000sccm, for example, it can be 100sccm, 200sccm, 300sccm, 400sccm, 500sccm, 600sccm, 700sccm, 800sccm, 900sccm or 1000sccm, but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0174] Among them, the coating speed of the growth of the IA group element layer is 0.1-1m / min, for example, it can be 0.1m / min, 0.1m / min, 0.2m / min, 0.3m / min, 0.4m / min, 0.5m / min, 0.6m / min, 0.7m / min, 0.8m / min, 0.9m / min or 1m / min, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0175] Among them, the thickness of the conductive layer obtained by growing the second conductive layer is 200-900nm, for example, it can be 200nm, 250nm, 300nm, 350nm, 400nm, 450nm, 500nm, 550nm, 600nm, 650nm, 700nm, 750nm, 800nm, 850nm or 900nm, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0176] Wherein, the second conductive layer is grown in a manner including: physical magnetron sputtering coating.

[0177] Among them, the power density of the growth of the second conductive layer is 2-6kW / m, for example, it can be 2kW / m, 2.5kW / m, 3kW / m, 3.5kW / m, 4kW / m, 4.5kW / m, 5kW / m, 5.5kW / m or 6kW / m, but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0178] Among them, the coating temperature for growing the second conductive layer is 50-150°C, for example, it can be 50°C, 60°C, 70°C, 80°C, 90°C, 100°C, 110°C, 120°C, 130°C, 140°C or 150°C, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0179] Among them, the coating pressure for the growth of the second conductive layer is 0.1-1Pa, for example, it can be 0.1Pa, 0.2Pa, 0.3Pa, 0.4Pa, 0.5Pa, 0.6Pa, 0.7Pa, 0.8Pa, 0.9Pa or 1Pa, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0180] Among them, the flow rate of argon gas in the growth of the second conductive layer is 100-500sccm, for example, it can be 100sccm, 150sccm, 200sccm, 250sccm, 300sccm, 350sccm, 400sccm, 450sccm or 500sccm, etc., but is not limited to the listed values. Other values ​​not listed in this range also meet the requirements.

[0181] Among them, the flow rate of oxygen in the growth of the second conductive layer is 0.1-1% of the total process gas flow, for example, it can be 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9% or 1%, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0182] Among them, the coating speed of the second conductive layer growth is 0.1-1m / min, for example, it can be 0.1m / min, 0.1m / min, 0.2m / min, 0.3m / min, 0.4m / min, 0.5m / min, 0.6m / min, 0.7m / min, 0.8m / min, 0.9m / min or 1m / min, etc., but is not limited to the listed values. Other values ​​not listed within this range also meet the requirements.

[0183] In the present invention, the total flow rate of process gas during the preparation of each layer refers to the total flow rate of argon and oxygen, and the control of specific concentrations can be achieved by regulating the flow rate of related gases during the process.

[0184] 3. This embodiment provides an electrochromic product, which includes: the electrochromic layer.

[0185] For example, the electrochromic product may be in the form of a vehicle rearview mirror, sunroof glass, car window glass, camouflage equipment, building window glass, etc.

[0186] 4. In order to illustrate the color changing effect that can be achieved by the electrochromic layer provided by the present invention, the following actual examples are used for illustration, as follows:

[0187] Example 1

[0188] This embodiment provides an electrochromic device, which is specifically as follows:

[0189] The method comprises: a first conductive layer, an insulating layer, a cathode electrochromic layer, an ion conducting layer, an anode electrochromic layer, an IA group element layer and a second conductive layer which are sequentially arranged on a substrate;

[0190] The substrate is glass with a thickness of 3 mm;

[0191] The first conductive layer is a FTO film layer with a thickness of 600 nm;

[0192] The isolation layer is a titanium oxide layer with a thickness of 75nm;

[0193] The cathode electrochromic layer is a tungsten oxide layer with a thickness of 300 nm;

[0194] The ion conducting layer is a silicon oxide layer with a thickness of 75 nm;

[0195] The anode electrochromic layer is a 240nm thick tungsten nickel tantalum oxide layer, and the target material used in the preparation is calculated by weight percentage: tungsten 40%, nickel 40%, and the balance is tantalum;

[0196] The Group IA element layer is a lithium layer with a thickness of 80 nm;

[0197] The second conductive layer is an ITO film layer with a thickness of 600 nm.

[0198] The preparation process is as follows:

[0199] The first conductive layer, the insulating layer, the cathode electrochromic layer, the ion conducting layer, the anode electrochromic layer, the IA group element layer and the second conductive layer are sequentially grown on the substrate;

[0200] The first conductive layer is grown by physical magnetron sputtering coating, with a power density of 3 kW / m, a coating temperature of 300° C., a coating pressure of 0.4 Pa, an argon flow rate of 400 sccm, an oxygen flow rate of 0.5% of the total process gas flow, and a coating speed of 0.5 m / min;

[0201] The insulating layer is grown by physical magnetron sputtering coating, with a power density of 10 kW / m, a coating temperature of 300°C, a coating pressure of 0.5 Pa, an argon flow rate of 500 sccm, an oxygen flow rate of 60% of the total process gas flow, and a coating speed of 0.5 m / min;

[0202] The cathode electrochromic layer is grown by physical magnetron sputtering with a power density of 15 kW / m, a coating temperature of 300° C., a coating pressure of 2 Pa, an argon flow rate of 500 sccm, an oxygen flow rate of 60% of the total process gas flow rate, and a coating speed of 0.5 m / min.

[0203] The ion conducting layer is grown by physical magnetron sputtering with a power density of 6 kW / m, a coating temperature of 40°C, a coating pressure of 2 Pa, an argon flow rate of 300 sccm, an oxygen flow rate of 90% of the total process gas flow rate, and a coating speed of 0.5 m / min.

[0204] The anode electrochromic layer is grown by physical magnetron sputtering with a power density of 15 kW / m, a coating temperature of 60° C., a coating pressure of 3 Pa, an argon flow rate of 300 sccm, an oxygen flow rate of 80% of the total process gas flow rate, and a coating speed of 0.5 m / min.

[0205] The IA group element layer is grown by physical magnetron sputtering with a power density of 6 kW / m, a coating temperature of 60° C., a coating pressure of 0.5 a, an argon flow rate of 800 sccm, and a coating speed of 0.5 m / min.

[0206] The second conductive layer is grown by physical magnetron sputtering coating with a power density of 5 kW / m, a coating temperature of 100°C, a coating pressure of 0.5 Pa, an argon flow rate of 300 sccm, an oxygen flow rate of 0.5% of the total process gas flow rate, and a coating speed of 0.5 m / min.

[0207] Example 2

[0208] This embodiment provides an electrochromic device, which is specifically as follows:

[0209] The method comprises: a first conductive layer, an insulating layer, a cathode electrochromic layer, an ion conducting layer, an anode electrochromic layer, an IA group element layer and a second conductive layer which are sequentially arranged on a substrate;

[0210] The substrate includes: glass with a thickness of 1 mm;

[0211] The first conductive layer is an ITO film layer with a thickness of 400 nm;

[0212] The isolation layer is a titanium oxide layer with a thickness of 50 nm;

[0213] The cathode electrochromic layer is a tungsten oxide layer with a thickness of 400 nm;

[0214] The ion conducting layer is a tungsten oxide layer with a thickness of 50 nm;

[0215] The anode electrochromic layer is a 300nm thick tungsten-nickel-tantalum oxide layer, and the target material used in the preparation comprises, by weight percentage, 42% tungsten, 38% nickel, and the balance tantalum;

[0216] The Group IA element layer is a potassium layer with a thickness of 120 nm;

[0217] The second conductive layer is an ITO film layer with a thickness of 400 nm.

[0218] The preparation process is as follows:

[0219] The first conductive layer, the insulating layer, the cathode electrochromic layer, the ion conducting layer, the anode electrochromic layer, the IA group element layer and the second conductive layer are sequentially grown on the substrate;

[0220] The first conductive layer is grown by physical magnetron sputtering coating, with a power density of 4 kW / m, a coating temperature of 325°C, a coating pressure of 0.6 Pa, an argon flow rate of 600 sccm, an oxygen flow rate of 0.3% of the total process gas flow, and a coating speed of 0.4 m / min;

[0221] The insulating layer is grown by physical magnetron sputtering coating, with a power density of 8 kW / m, a coating temperature of 280°C, a coating pressure of 0.6 Pa, an argon flow rate of 300 sccm, an oxygen flow rate of 40% of the total process gas flow, and a coating speed of 0.6 m / min;

[0222] The cathode electrochromic layer is grown by physical magnetron sputtering with a power density of 18 kW / m, a coating temperature of 340°C, a coating pressure of 1 Pa, an argon flow rate of 600 sccm, an oxygen flow rate of 80% of the total process gas flow, and a coating speed of 0.6 m / min.

[0223] The ion conducting layer is grown by physical magnetron sputtering with a power density of 8 kW / m, a coating temperature of 60°C, a coating pressure of 3 Pa, an argon flow rate of 200 sccm, an oxygen flow rate of 75% of the total process gas flow rate, and a coating speed of 0.3 m / min.

[0224] The anode electrochromic layer is grown by physical magnetron sputtering with a power density of 12 kW / m, a coating temperature of 80° C., a coating pressure of 2 Pa, an argon flow rate of 100 sccm, an oxygen flow rate of 90% of the total process gas flow rate, and a coating speed of 0.3 m / min.

[0225] The IA group element layer is grown by physical magnetron sputtering with a power density of 8 kW / m, a coating temperature of 40° C., a coating pressure of 0.5 Pa, an argon flow rate of 500 sccm, and a coating speed of 0.8 m / min.

[0226] The second conductive layer is grown by physical magnetron sputtering coating with a power density of 3kW / m, a coating temperature of 125°C, a coating pressure of 0.8Pa, an argon flow rate of 400sccm, an oxygen flow rate of 0.3% of the total process gas flow rate, and a coating speed of 0.6m / min.

[0227] Example 3

[0228] This embodiment provides an electrochromic device, which is specifically as follows:

[0229] The method comprises: a first conductive layer, an insulating layer, a cathode electrochromic layer, an ion conducting layer, an anode electrochromic layer, an IA group element layer and a second conductive layer which are sequentially arranged on a substrate;

[0230] The substrate is glass with a thickness of 5 mm;

[0231] The first conductive layer is a FTO film layer with a thickness of 900 nm;

[0232] The isolation layer is a titanium oxide layer with a thickness of 100 nm;

[0233] The cathode electrochromic layer is a tungsten oxide layer with a thickness of 500 nm;

[0234] The ion conducting layer is a silicon oxide layer with a thickness of 100 nm;

[0235] The anode electrochromic layer is a 500nm thick tungsten nickel titanium oxide layer, and the target material used in the preparation comprises, by weight percentage, 35% tungsten, 35% nickel, and the balance titanium;

[0236] The IA group element layer is a lithium layer and a sodium layer, and has a thickness of 150 nm;

[0237] The second conductive layer is an ITO film layer with a thickness of 900 nm.

[0238] The preparation process is as follows:

[0239] The first conductive layer, the insulating layer, the cathode electrochromic layer, the ion conducting layer, the anode electrochromic layer, the IA group element layer and the second conductive layer are sequentially grown on the substrate;

[0240] The first conductive layer is grown by physical magnetron sputtering coating with a power density of 5 kW / m, a coating temperature of 250° C., a coating pressure of 0.1 Pa, an argon flow rate of 200 sccm, an oxygen flow rate of 0.6% of the total process gas flow, and a coating speed of 0.1 m / min.

[0241] The insulating layer is grown by physical magnetron sputtering coating, with a power density of 15 kW / m, a coating temperature of 250°C, a coating pressure of 0.3 Pa, an argon flow rate of 50 sccm, an oxygen flow rate of 80% of the total process gas flow, and a coating speed of 0.1 m / min;

[0242] The cathode electrochromic layer is grown by physical magnetron sputtering with a power density of 10 kW / m, a coating temperature of 380° C., a coating pressure of 0.5 Pa, an argon flow rate of 1000 sccm, an oxygen flow rate of 50% of the total process gas flow, and a coating speed of 1 m / min.

[0243] The ion conducting layer is grown by physical magnetron sputtering, with a power density of 10 kW / m, a coating temperature of 30° C., a coating pressure of 0.5 Pa, an argon flow rate of 0 sccm, an oxygen flow rate of 100% of the total process gas flow rate, and a coating speed of 1 m / min.

[0244] The anode electrochromic layer is grown by physical magnetron sputtering with a power density of 10 kW / m, a coating temperature of 100° C., a coating pressure of 4 Pa, an argon flow rate of 500 sccm, an oxygen flow rate of 60% of the total process gas flow rate, and a coating speed of 1 m / min.

[0245] The IA group element layer is grown by physical magnetron sputtering with a power density of 10 kW / m, a coating temperature of 30° C., a coating pressure of 0.1 Pa, an argon flow rate of 1000 sccm, and a coating speed of 0.1 m / min.

[0246] The second conductive layer is grown by physical magnetron sputtering coating with a power density of 2 kW / m, a coating temperature of 50°C, a coating pressure of 0.1 Pa, an argon flow rate of 100 sccm, an oxygen flow rate of 1% of the total process gas flow, and a coating speed of 0.1 m / min.

[0247] Example 4

[0248] This embodiment provides an electrochromic device, which is specifically as follows:

[0249] The method comprises: a first conductive layer, an insulating layer, a cathode electrochromic layer, an ion conducting layer, an anode electrochromic layer, an IA group element layer and a second conductive layer which are sequentially arranged on a substrate;

[0250] The substrate is glass with a thickness of 0.4 mm;

[0251] The first conductive layer is an ITO film layer with a thickness of 100 nm;

[0252] The isolation layer is a titanium oxide layer with a thickness of 25 nm;

[0253] The cathode electrochromic layer is a tungsten oxide layer with a thickness of 200 nm;

[0254] The ion conducting layer is a tungsten oxide layer with a thickness of 25 nm;

[0255] The anode electrochromic layer is a 200nm thick tungsten-nickel-molybdenum oxide layer, and the target material used in the preparation comprises, by weight percentage, 45% tungsten, 45% nickel, and the balance molybdenum;

[0256] The Group IA element layer is a lithium layer with a thickness of 50 nm;

[0257] The second conductive layer is an ITO film layer with a thickness of 200 nm.

[0258] The preparation process is as follows:

[0259] The first conductive layer, the insulating layer, the cathode electrochromic layer, the ion conducting layer, the anode electrochromic layer, the IA group element layer and the second conductive layer are sequentially grown on the substrate;

[0260] The first conductive layer is grown by physical magnetron sputtering coating, with a power density of 2 kW / m, a coating temperature of 350° C., a coating pressure of 0.1 Pa, an argon flow rate of 800 sccm, an oxygen flow rate of 0.1% of the total process gas flow, and a coating speed of 1 m / min;

[0261] The insulating layer is grown by physical magnetron sputtering coating, with a power density of 5 kW / m, a coating temperature of 350°C, a coating pressure of 0.8 Pa, an argon flow rate of 1000 sccm, an oxygen flow rate of 30% of the total process gas flow, and a coating speed of 1 m / min;

[0262] The cathode electrochromic layer is grown by physical magnetron sputtering with a power density of 20 kW / m, a coating temperature of 250° C., a coating pressure of 4 Pa, an argon flow rate of 0 sccm, an oxygen flow rate of 100% of the total process gas flow rate, and a coating speed of 0.1 m / min.

[0263] The ion conducting layer is grown by physical magnetron sputtering with a power density of 5 kW / m, a coating temperature of 80°C, a coating pressure of 4 Pa, an argon flow rate of 500 sccm, an oxygen flow rate of 65% of the total process gas flow rate, and a coating speed of 0.1 m / min.

[0264] The anode electrochromic layer is grown by physical magnetron sputtering, with a power density of 20 kW / m, a coating temperature of 30° C., a coating pressure of 4 Pa, an argon flow rate of 0 sccm, an oxygen flow rate of 100% of the total process gas flow rate, and a coating speed of 0.1 m / min.

[0265] The IA group element layer is grown by physical magnetron sputtering with a power density of 2 kW / m, a coating temperature of 80° C., a coating pressure of 1 Pa, an argon flow rate of 100 sccm, and a coating speed of 1 m / min.

[0266] The second conductive layer is grown by physical magnetron sputtering coating with a power density of 6 kW / m, a coating temperature of 150°C, a coating pressure of 1 Pa, an argon flow rate of 500 sccm, an oxygen flow rate of 0.1% of the total process gas flow, and a coating speed of 0.1 m / min.

[0267] Comparative Example 1

[0268] The only difference from Example 1 is that the target material used in preparing the anode electrochromic layer contains 50% tungsten and 50% nickel by mass.

[0269] Comparative Example 2

[0270] The only difference from Example 1 is that the target material used in preparing the anode electrochromic layer contains, by mass percentage, 40% tungsten, 40% nickel, and the remainder niobium.

[0271] Example 5

[0272] The only difference from Example 1 is that the cathode electrochromic layer is replaced with W of equal thickness. 0.80 Ti 0.10 Mo 0.10 O3.

[0273] Example 6

[0274] The only difference from Example 1 is that the target material used in preparing the anode electrochromic layer contains, by mass percentage, 20% tungsten, 40% nickel, and the balance tantalum.

[0275] Example 7

[0276] The only difference from Example 1 is that the target material used in preparing the anode electrochromic layer contains, by mass percentage, 50% tungsten, 40% nickel, and the remainder tantalum.

[0277] Example 8

[0278] The only difference from Example 1 is that the target material used in preparing the anode electrochromic layer contains, by mass percentage, 40% tungsten, 20% nickel, and the remainder tantalum.

[0279] Example 9

[0280] The only difference from Example 1 is that the target material used in preparing the anode electrochromic layer contains, by mass percentage, 40% tungsten, 50% nickel, and the remainder tantalum.

[0281] The electrochromic devices obtained in the above examples and comparative examples were tested for color change performance. Specifically, a voltage was applied to the electrochromic product until the device faded to a transparent state and the transmittance b value was measured using a transmittance measuring instrument. The results are shown in Table 1 below. The photos of the electrochromic devices obtained in Example 1 and Comparative Example 1 in the faded state are shown in Table 1 below. Figure 2 and Figure 3 shown.

[0282] Table 1

[0283]

[0284]

[0285] From Table 1 and Figure 2 and Figure 3 It can be seen that the electrochromic device provided by the present invention can achieve a transparent effect when fading without the problem of yellowing by optimizing the components within the electrochromic device, especially the anode electrochromic layer.

[0286] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the scope of protection of the present invention.

[0287] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any appropriate manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

[0288] In addition, the various embodiments of the present invention may be arbitrarily combined, and as long as they do not violate the concept of the present invention, they should also be regarded as the contents disclosed by the present invention.

Claims

1. An electrochromic device, characterized in that: The electrochromic device comprises: a first conductive layer, an insulating layer, a cathode electrochromic layer, an ion conducting layer, an anode electrochromic layer, an IA group element layer and a second conductive layer sequentially arranged on a substrate; The anode electrochromic layer includes tungsten nickel oxide X oxide, where X includes one or a combination of at least two of tantalum, titanium or molybdenum.

2. The electrochromic device according to claim 1, wherein The substrate comprises: glass with a thickness of 0.4-5 mm; Preferably, the first conductive layer includes: an ITO film layer and / or a FTO film layer; Preferably, the thickness of the first conductive layer is 100-900 nm.

3. The electrochromic device according to claim 1 or 2, characterized in that: The insulating layer includes: a titanium oxide layer; Preferably, the thickness of the insulating layer is 25-100 nm.

4. The electrochromic device according to any one of claims 1 to 3, characterized in that: The cathode electrochromic layer includes: a tungsten oxide layer; Preferably, the cathode electrochromic layer has a thickness of 200-500 nm.

5. The electrochromic device according to any one of claims 1 to 4, characterized in that: The ion conducting layer comprises: one of a tungsten oxide layer, a silicon oxide layer, a silicon aluminum oxide layer or a tungsten nickel oxide layer; Preferably, the thickness of the ion conducting layer is 25-100 nm.

6. The electrochromic device according to any one of claims 1 to 5, characterized in that: The target material used in the preparation of the anode electrochromic layer comprises, by weight percentage, 35-45% tungsten, 35-45% nickel, and the balance X; Preferably, the thickness of the anode electrochromic layer is 200-500 nm; Preferably, the Group IA element layer comprises: one of a lithium layer, a sodium layer or a potassium layer; Preferably, the thickness of the Group IA element layer is 50-150 nm.

7. The electrochromic device according to any one of claims 1 to 6, characterized in that: The second conductive layer includes: an ITO film layer; Preferably, the thickness of the second conductive layer is 200-900 nm.

8. A method for preparing an electrochromic device, characterized in that: The preparation method comprises: sequentially growing a first conductive layer, an insulating layer, a cathode electrochromic layer, an ion conducting layer, an anode electrochromic layer, a group IA element layer and a second conductive layer on a substrate.

9. The preparation method according to claim 8, wherein The thickness of the conductive layer obtained by growing the first conductive layer is 100-900 nm; Preferably, the first conductive layer is grown by: physical magnetron sputtering coating; Preferably, the power density of the growth of the first conductive layer is 2-5 kW / m; Preferably, the coating temperature for growing the first conductive layer is 250-350°C; Preferably, the coating pressure for growing the first conductive layer is 0.1-0.8 Pa; Preferably, the flow rate of argon gas during the growth of the first conductive layer is 200-800 sccm; Preferably, the flow rate of oxygen during the growth of the first conductive layer is 0.1-0.6% of the total process gas flow; Preferably, the coating speed of the first conductive layer is 0.1-1 m / min; Preferably, the thickness of the insulating layer obtained by growing the insulating layer is 25-100 nm; Preferably, the method of growing the insulating layer includes: physical magnetron sputtering coating; Preferably, the power density of the insulating layer growth is 5-15 kW / m; Preferably, the coating temperature for the growth of the insulating layer is 250-350°C; Preferably, the coating pressure for the growth of the insulating layer is 0.3-0.8 Pa; Preferably, the flow rate of argon gas during the growth of the isolation layer is 50-1000 sccm; Preferably, the flow rate of oxygen in the growth of the insulating layer is 30-80% of the total process gas flow; Preferably, the coating speed of the insulating layer growth is 0.1-1 m / min; Preferably, the thickness of the conductive layer obtained by growing the cathode electrochromic layer is 200-500 nm; Preferably, the cathode electrochromic layer is grown by: physical magnetron sputtering coating; Preferably, the power density of the cathode electrochromic layer growth is 10-20 kW / m; Preferably, the coating temperature for growing the cathode electrochromic layer is 250-380°C; Preferably, the coating pressure for growing the cathode electrochromic layer is 0.5-4 Pa; Preferably, the flow rate of argon gas during the growth of the cathode electrochromic layer is ≤1000 sccm; Preferably, the flow rate of oxygen during the growth of the cathode electrochromic layer is 50-100% of the total process gas flow; Preferably, the coating speed of the cathode electrochromic layer is 0.1-1 m / min; Preferably, the thickness of the ion conducting layer obtained by growing the ion conducting layer is 25-100 nm; Preferably, the ion conducting layer is grown by: physical magnetron sputtering coating; Preferably, the power density of the ion conducting layer growth is 5-10 kW / m; Preferably, the coating temperature for the growth of the ion conducting layer is 30-80°C; Preferably, the coating pressure for the growth of the ion conductive layer is 0.5-4 Pa; Preferably, the flow rate of argon gas during the growth of the ion conducting layer is ≤500 sccm; Preferably, the flow rate of oxygen during the growth of the ion conducting layer is 65-100% of the total process gas flow; Preferably, the coating speed of the ion conductive layer is 0.1-1 m / min; Preferably, the thickness of the conductive layer obtained by growing the anode electrochromic layer is 200-500 nm; Preferably, the anode electrochromic layer is grown by: physical magnetron sputtering coating; Preferably, the power density of the growth of the anode electrochromic layer is 10-20 kW / m; Preferably, the coating temperature for growing the anode electrochromic layer is 30-100°C; Preferably, the coating pressure for growing the anode electrochromic layer is 0.5-4 Pa; Preferably, the flow rate of argon gas during the growth of the anode electrochromic layer is ≤500 sccm; Preferably, the flow rate of oxygen during the growth of the anode electrochromic layer is 60-100% of the total process gas flow; Preferably, the coating speed of the anode electrochromic layer is 0.1-1 m / min; Preferably, the thickness of the conductive layer obtained by growing the Group IA element layer is 50-150 nm; Preferably, the method of growing the group IA element layer includes: physical magnetron sputtering coating; Preferably, the power density of the growth of the group IA element layer is 2-10 kW / m; Preferably, the coating temperature for growing the group IA element layer is 30-80°C; Preferably, the coating pressure for growing the group IA element layer is 0.1-1 Pa; Preferably, the flow rate of argon gas during the growth of the Group IA element layer is 100-1000 sccm; Preferably, the coating speed of the IA group element layer is 0.1-1 m / min; Preferably, the thickness of the conductive layer obtained by growing the second conductive layer is 200-900 nm; Preferably, the second conductive layer is grown by: physical magnetron sputtering coating; Preferably, the power density of the growth of the second conductive layer is 2-6 kW / m; Preferably, the coating temperature for growing the second conductive layer is 50-150°C; Preferably, the coating pressure for growing the second conductive layer is 0.1-1 Pa; Preferably, the flow rate of argon gas during the growth of the second conductive layer is 100-500 sccm; Preferably, the flow rate of oxygen during the growth of the second conductive layer is 0.1-1% of the total process gas flow; Preferably, the coating speed of the second conductive layer is 0.1-1 m / min.

10. An electrochromic product, characterized in that: The electrochromic product comprises the electrochromic layer according to any one of claims 1 to 7.

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