CN112099277A

CN112099277A - Electrochromic assembly structure with protective layer

Info

Publication number: CN112099277A
Application number: CN201910526267.7A
Authority: CN
Inventors: 钟仪文
Original assignee: Tintable Kibing Co ltd
Current assignee: Tintable Kibing Co ltd
Priority date: 2019-06-18
Filing date: 2019-06-18
Publication date: 2020-12-18

Abstract

The invention relates to an electrochromic component structure with a protective layer, which is formed with a first substrate, a first transparent conducting layer, a first electrochromic layer, a protective layer, an electrolyte layer, a second electrochromic layer, a second transparent conducting layer and a second substrate in sequence, wherein the protective layer is made of tin oxide (SnO)_x) Or nickel oxide (NiO)_x) (ii) a Therefore, the protective layer can improve the gluing characteristic of the first electrochromic layer and the electrolyte layer, and improve the acid-base resistance and the environment resistance of the first electrochromic layer.

Description

Electrochromic assembly structure with protective layer

Technical Field

The present invention relates to an electrochromic device structure, and more particularly, to an electrochromic device structure with a protective layer, wherein the protective layer is additionally disposed between an electrochromic layer and an electrolyte layer, so as to improve acid-base resistance and environmental resistance of the electrochromic layer, and provide a good bonding effect between the electrochromic layer and the electrolyte layer.

Background

The electrochromic technology utilizes the optical characteristics of the material, and under the action of an external electric field, the material generates a color change phenomenon, and the color and the transparency of the material are reversibly changed in appearance. At present, the application range of the electrochromic technology is quite wide, the industries such as vehicles, military, buildings and the like can use the electrochromic technology, and the industries such as rearview mirrors and skylights of the vehicles, the camouflage function of the military and windows in the buildings can use the electrochromic technology to achieve different purposes.

Materials used in the electrochromic technology mostly use Prussian Blue (Prussian Blue), vanadium pentoxide, tungsten oxide, nickel oxide, molybdenum oxide, titanium oxide, cobalt oxide and the like; the electrochromic device is generally a sandwich-type layered structure, the outermost two-layer structure adopts glass or plastic as a substrate, and a transparent conductive layer, an electrochromic layer, an ion storage layer, an electrolyte layer and other structures are formed in the middle.

Taiwan patent publication No. TW I60515 (electrochromic device and method for manufacturing the same) provides an electrochromic device structure, which includes a substrate, a first transparent conductive layer, a first electrochromic material layer, an ion conductive layer, a second electrochromic material layer, and a second transparent conductive layer. Also, taiwan patent No. TW I534518 (electrochromic device) provides an electrochromic device including an electrochromic element, and the electrochromic element includes two substrates disposed opposite to each other, two transparent conductive layers respectively disposed on the two substrates, an ion conductor layer disposed between the two transparent conductive layers, an electrochromic layer disposed between the ion conductor layer and one of the transparent conductive layers, and an ion storage layer disposed between the ion conductor layer and the other transparent conductive layer.

From the above patent, it is known that the electrochromic layer of the electrochromic device is usually disposed adjacent to the electrolyte layer (ion conducting layer, ion conductor layer), but due to the relationship of the selected materials, the structural disposition leads to better adhesion between the electrolyte layer and the second electrochromic material layer, and thus poorer adhesion between the electrolyte layer and the first electrochromic material layer; moreover, if the first electrochromic material layer is made of tungsten oxide, although tungsten oxide has good electrochemical properties, the resistance to acid and alkali and the resistance to environment are very poor, so that the first electrochromic material layer is easily hydrolyzed.

Therefore, how to provide a structure capable of improving the adhesion property between the electrolyte layer and the electrochromic layer and simultaneously improving the acid and alkali resistance and the environmental resistance of the assembly is the direction the inventor thinks.

Disclosure of Invention

The invention mainly aims to provide an electrochromic assembly structure with a protective layer, which improves the bonding characteristic between a first electrochromic layer and an electrolyte layer by additionally arranging the protective layer, so that the electrolyte layer can still keep good adhesion to the first electrochromic layer, and the acid-base resistance and environment resistance of the electrochromic assembly are improved by the characteristics of the protective layer, and the protective layer also has good electrochemical characteristics and ion conduction characteristics.

In order to achieve the above-mentioned objectives, the present invention provides an electrochromic device structure with a protection layer, which sequentially comprises a first substrate, a first transparent conductive layer, a first electrochromic layer, a protection layer, an electrolyte layer, a second electrochromic layer, a second transparent conductive layer and a second substrate, wherein the protection layer is made of tin oxide (SnO)_x) Or nickel oxide (NiO)_x)。

In one embodiment of the present invention, the first electrochromic layer is made of tungsten oxide (WO)₃) And is prepared by an electron gun evaporation method (E-beam evaporation), an Ion-beam Assisted evaporation (IAD) method or a Sputtering method (Sputtering).

In an embodiment of the invention, the second electrochromic layer is made of nickel oxide (NiO) and is prepared by an electron gun evaporation method (E-beam evaporation), an Ion-beam Assisted evaporation (IAD) method, or a Sputtering method (Sputtering).

In one embodiment of the present invention, tin oxide (SnO)_x) X of 1.5-2.5, nickel oxide (NiO)_x) X of (b) is 0.5-1.5.

In one embodiment of the present invention, the surface roughness of the passivation layer is 5nm to 40 nm.

In one embodiment of the present invention, the thickness of the passivation layer is 25nm to 150 nm.

In an embodiment of the invention, the passivation layer is prepared by using an electron-gun evaporation method (E-beam evaporation), an Ion-Assisted evaporation (IAD) method Assisted by an electron-gun evaporation method, or Sputtering (Sputtering).

Drawings

Fig. 1 is a schematic structural diagram of a preferred embodiment of the present invention.

FIG. 2 is a line drawing illustrating roughness of tungsten oxide according to a preferred embodiment of the present invention.

FIG. 3 is a line graph showing roughness of nickel oxide according to a preferred embodiment of the present invention.

FIG. 4 is a schematic diagram of a surface structure of a tin oxide passivation layer according to a preferred embodiment of the present invention.

FIG. 5 is a schematic diagram of a surface structure of a nickel oxide passivation layer according to a preferred embodiment of the present invention.

Description of the symbols

1 first substrate 2 first transparent conductive layer

3 first electrochromic layer 4 protective layer

5 electrolyte layer 6 second electrochromic layer

7 second transparent conductive layer 8 second substrate

Detailed Description

The purpose of the present invention and its structural and functional advantages will be described with reference to the following figures and embodiments.

Referring to fig. 1, the present invention provides an electrochromic device structure with a protective layer, which sequentially comprises a first substrate 1, a first transparent conductive layer 2, a first electrochromic layer 3, a protective layer 4, an electrolyte layer 5, a second electrochromic layer 6, a second transparent conductive layer 7 and a second substrate 8, wherein the protective layer 4 is prepared by electron gun evaporation, electron gun evaporation with ion-assisted evaporation or sputtering, and tin oxide (SnO) is selected_x) Or nickel oxide (NiO)_x) As a material, tin oxide (SnO)_x) X of 1.5-2.5, nickel oxide (NiO)_x) X of (2) is 0.5-1.5, and the surface roughness is 5-40 nm, and the thickness is 25-150 nm;

wherein, the first electrochromic layer 3 is made of tungsten oxide (WO)₃) The second electrochromic layer 6 is made of nickel oxide (NiO), and the first electrochromic layer 3 and the second electrochromic layer 6 are made of nickel oxide (NiO)It is also prepared by electron gun evaporation, electron gun evaporation with ion assisted evaporation or sputtering.

Further, the scope of practical application of the present invention will be further demonstrated by the following specific examples, which are not intended to limit the scope of the invention in any way.

With reference to fig. 1, the present invention provides an electrochromic device structure with a protective layer, which has a first substrate 1 and a second substrate 8 disposed opposite to each other, and is made of glass or plastic, wherein the first substrate 1 is sequentially formed with a first transparent conductive layer 2, a first electrochromic layer 3, a protective layer 4, an electrolyte layer 5, a second electrochromic layer 6, and a second transparent conductive layer 7, and finally the second transparent conductive layer 7 is covered with the second substrate 8 to complete the electrochromic device.

In practical implementation of the present invention, after the first transparent conductive layer 2 is plated on the first substrate 1, the first substrate is placed in an evaporation machine, vacuum pumping is performed to a designated process pressure, an ion gun is then turned on to remove static electricity and dust in a cavity of the evaporation machine, and then, after process gas oxygen is introduced, the oxygen flow is 200-350sccm, the electron gun is turned on to perform electron gun evaporation, and an ion-assisted evaporation is used to perform evaporation, and an ion source-assisted evaporation process is used to form tungsten oxide (WO) on the first transparent conductive layer 2₃) A thin film, i.e., the first electrochromic layer 3;

after the first electrochromic layer 3 is evaporated to a specified thickness, the electron gun evaporation method and the ion assisted evaporation method are also used to prepare the protection layer 4, wherein tin oxide or nickel oxide can be selected, the oxygen flow rate is set to 200-400sccm, and the protection layer 4 is formed to be tin oxide (SnO) with a thickness of 25-150 nm_x) Thin film or nickel oxide (NiO) with thickness of 25nm-150nm_x) And (5) finishing the preparation process of the protective layer 4. In this way, the protection layer 4 is formed between the first electrochromic layer 3 and the electrolyte layer 5, so that the first electrochromic layer 3 and the electrolyte layer 5 have good bonding characteristics, thereby improving the reliability of the electrochromic device.

The protective layer 4 was analyzed by an X-ray energy dispersive spectrometer (EDX), which showed thatTin oxide (SnO) of the protective layer 4_x) Has an oxygen atom ratio x of 1.5-2.5, and nickel oxide (NiO)_x) The oxygen atom ratio x of the film is between 0.5 and 1.5.

In addition, in order to increase the bonding characteristic, in practice, rough surfaces are manufactured on the first electrochromic layer 3 and the protective layer 4, and the surface roughness of the first electrochromic layer 3 and the protective layer 4 is measured by a surface profiler (α -step);

referring to fig. 2, which shows the surface roughness of the first electrochromic layer 3, 64 test pieces were fabricated in this example, and the first electrochromic layer 3 was made of tungsten oxide according to the results measured by a surface profiler (WO)₃) The surface roughness average of the material is about 0.0108 μm;

and the protective layer 4 is tin oxide (SnO)_x) Film and nickel oxide (NiO)_x) Thin film, first, tin oxide (SnO)_x) The surface roughness of the film can be referred to in table 1 below:

TABLE 1

Oxygen flow (sccm)	50	100	150	200	250
						Roughness (μm)	0.0236	0.0281	0.0243	0.0301	0.0291

As can be seen from the results measured by the surface profiler in Table 1, the surface roughness varies according to the flow rate of oxygen introduced by the electron gun evaporation method and the ion assisted evaporation method, and the protective layer 4 is tin oxide (SnO)_x) The surface roughness average of the film was about 0.027 μm; if the protective layer 4 is nickel oxide (NiO)_x) Film, as measured by the surface profiler, see FIG. 3, protective layer 4 was nickel oxide (NiO)_x) The surface roughness of the film averaged about 0.0102 μm, with an oxygen flow of 350 sccm.

Referring to fig. 4 and 5, which are surface structures of the protective layer 4 formed on the first electrochromic layer 3, images observed by using a scanning electron microscope are shown, and fig. 4 is tin oxide (SnO)_x) Surface structure of the film, nickel oxide (NiO) in FIG. 5_x) The surface structure of the film, tin oxide (SnO), is clearly shown_x) With nickel oxide (NiO)_x) The protective layers 4 are all made to be uneven surfaces.

As can be seen from the above description, the present invention has the following advantages compared with the prior art:

1. compared with the prior structure, the electrochromic assembly structure with the protective layer has the advantages that the protective layer is formed between the first electrochromic layer and the electrolyte layer, and the electrolyte layer is biased to be attached to the second electrochromic layer.

2. The invention provides an electrochromic component structure with a protective layer, wherein the protective layer is made of tin oxide (SnO)_x) Or nickel oxide (NiO)_x) Formed on the first electrochromic layer, can improve tungsten oxide (WO)₃) The protective layer may promote the first electrochromic layerThe first electrochromic layer is not easy to corrode or hydrolyze due to the acid and alkali resistance and environmental resistance, and the service life of the electrochromic assembly can be effectively prolonged.

Claims

1. An electrochromic component structure with a protective layer is sequentially formed with a first substrate, a first transparent conductive layer, a first electrochromic layer, a protective layer, an electrolyte layer, a second electrochromic layer, a second transparent conductive layer and a second substrate, wherein the protective layer is made of tin oxide SnO_xOr nickel oxide NiO_x。

2. The protected electrochromic assembly structure of claim 1, wherein the first electrochromic layer is tungsten oxide WO₃And is prepared by an electron gun evaporation method, an electron gun evaporation method and an ion-assisted evaporation method or a sputtering method.

3. The electrochromic device structure with a protective layer according to claim 1, wherein the second electrochromic layer is made of NiO and is prepared by electron gun deposition, electron gun deposition with ion assisted deposition, or sputtering.

4. The protected electrochromic assembly structure of claim 1 wherein said tin oxide SnO_xX of (b) is 1.5 to 2.5, and the nickel oxide NiO_xX of (b) is 0.5-1.5.

5. The electrochromic device structure with protective layer according to claim 1, wherein the surface roughness of the protective layer is 5nm to 40 nm.

6. The electrochromic device structure with protective layer according to claim 1, wherein the protective layer has a thickness of 25nm to 150 nm.

7. The electrochromic device structure with a protective layer of claim 1, wherein the protective layer is formed by electron gun evaporation, electron gun evaporation with ion assisted evaporation, or sputtering.