CN110737143A - all-solid-state electrochromic devices with quick response and preparation method thereof - Google Patents
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Abstract
fast-response all-solid-state electrochromic devices and a preparation method thereof, which relate to electrochromic devices and a preparation method thereof, the invention aims to solve the problems of low preparation efficiency and low response speed of the existing electrochromic devices. fast-response all-solid-state electrochromic devices comprise a substrate, a bottom electrode layer, an electrochromic layer, a complementary electrochromic layer, a lithium layer and a top electrode layer.
Description
Technical Field
The invention relates to electrochromic devices and a preparation method thereof.
Background
The electrochromic materials are various in types and mainly divided into organic electrochromic materials such as conducting polymers, organic micromolecular dyes and the like and inorganic electrochromic materials such as transition metal oxides, metal coordination complexes and the like, and the electrochromic materials have -wide application potential in the fields of intelligent windows, anti-dazzling rearview mirrors, aerospace thermal control, aircraft windows and the like.
The traditional all-solid-state electrochromic device generally comprises a five-layer structure of a bottom electrode layer, an electrochromic layer, an electrolyte layer or an ion conducting layer, an ion storage layer or a complementary electrochromic layer and a top electrode layer, at present, lithium-containing inorganic salt is generally adopted for providing color-changing ions for the electrolyte layer of the electrochromic device, but the electrolyte layer reduces the preparation efficiency in the aspect of , in addition, in the aspect of , the internal resistance of the whole device is larger, the ion transmission efficiency is reduced, and the response speed of the device is reduced.
Disclosure of Invention
The invention aims to solve the problems of low preparation efficiency and low response speed of the conventional electrochromic device, and provides all-solid-state electrochromic devices with quick response and a preparation method thereof.
The fast-response all-solid-state electrochromic device comprises a substrate, a bottom electrode layer, an electrochromic layer, a complementary color-changing layer, a lithium layer and a top electrode layer, wherein the bottom electrode layer, the electrochromic layer, the complementary color-changing layer and the top electrode layer are sequentially arranged on the substrate from bottom to top or the bottom electrode layer, the complementary color-changing layer, the electrochromic layer and the top electrode layer are sequentially arranged on the substrate from bottom to top, and the lithium layer is distributed in the electrochromic layer and the complementary color-changing layer.
The preparation method of kinds of fast-response all-solid-state electrochromic devices is completed according to the following steps:
, which adopts the following four methods to prepare the fast response all-solid-state electrochromic device:
method comprises sequentially depositing a bottom electrode layer, an electrochromic layer, a complementary electrochromic layer, a lithium layer and a top electrode layer on a substrate by vacuum coating, magnetron sputtering, vacuum thermal evaporation or electron beam evaporation;
the second method comprises the following steps: sequentially depositing a bottom electrode layer, an electrochromic layer, a lithium layer, a complementary electrochromic layer and a top electrode layer on a substrate by adopting a vacuum coating method, a magnetron sputtering method, a vacuum thermal evaporation method or an electron beam evaporation method;
the third method comprises the following steps: sequentially depositing a bottom electrode layer, a complementary color changing layer, an electrochromic layer, a lithium layer and a top electrode layer on a substrate by adopting a vacuum coating method, a magnetron sputtering method, a vacuum thermal evaporation method or an electron beam evaporation method;
the method four comprises the following steps: and sequentially depositing a bottom electrode layer, a complementary color changing layer, a lithium layer, an electrochromic layer and a top electrode layer on the substrate by adopting a vacuum coating method, a magnetron sputtering method, a vacuum thermal evaporation method or an electron beam evaporation method.
The principle and the advantages of the invention are as follows:
, novel fast-response all-solid-state electrochromic device structures can be obtained, the structures comprise four layers of structures, namely a bottom electrode layer, an electrochromic layer, a complementary electrochromic layer and a top electrode layer, and color-changing ions are introduced by directly sputtering or evaporating metal lithium, and lithium diffuses into the electrochromic layer and the complementary electrochromic layer in the preparation process and does not exist independently due to small lithium atom radius;
secondly, the fast-response all-solid-state electrochromic devices prepared by the method can realize color change by applying voltage after the preparation is finished, and can also carry out heat treatment to optimize the color change function, wherein the heat treatment is carried out in vacuum, atmospheric atmosphere or inert gas atmosphere;
and thirdly, the fast-response all-solid-state electrochromic devices do not need an intermediate electrolyte layer or an ion conducting layer, so that the production cost can be reduced, the preparation efficiency can be improved, and the internal impedance of the devices can be reduced, therefore, the performance of the devices is superior to that of electrochromic devices with electrolyte layer or ion conducting layer structures, and the response time is less than 5 seconds.
The present invention can obtain kinds of fast response all-solid electrochromic devices.
Drawings
FIG. 1 is a cross-sectional SEM image of fast response all-solid-state electrochromic devices prepared in example ;
fig. 2 is a graph of the response times of fast responding all-solid-state electrochromic devices prepared in example .
Detailed Description
Specific embodiment , the fast response all-solid-state electrochromic device comprises a substrate, a bottom electrode layer, an electrochromic layer, a complementary color-changing layer, a lithium layer and a top electrode layer, wherein the bottom electrode layer, the electrochromic layer, the complementary color-changing layer and the top electrode layer are arranged on the substrate in sequence from bottom to top, or the bottom electrode layer, the complementary color-changing layer, the electrochromic layer and the top electrode layer are arranged on the substrate in sequence from bottom to top, and the lithium layer is distributed in the electrochromic layer and the complementary color-changing layer.
The second embodiment is different from the second embodiment in that the substrate is a heat-resistant substrate or a flexible substrate, the heat-resistant substrate is glass, the flexible substrate is polyethylene terephthalate or polydimethylsiloxane, and other steps are the same as those in embodiment .
The third embodiment is different from the embodiment in that the bottom electrode layer is an ito layer, an oxyfluoride-doped sn layer, or a metal layer, the metal is ag, au, or pt, and other steps are the same as those in the third embodiment or the second embodiment.
Fourth embodiment of this embodiment is different from embodiments to in that the electrochromic layer is a tungsten oxide layer or a vanadium oxide layer, the tungsten oxide has a tungsten-to-oxygen ratio of 1 (1 to 3), and other steps are the same as those in embodiments to iii.
Fifth embodiment of this embodiment is different from embodiments to forty in that the complementary discoloration layer includes a nickel oxide layer, a vanadium oxide layer, a tantalum oxide layer, a titanium oxide layer, a cobalt oxide layer, a zirconium oxide layer, an yttrium oxide layer, and a nickel tungsten oxide layer, the amount of tungsten doped in the nickel tungsten oxide layer is 1% to 50%, and other steps are the same as in embodiments to forty.
Sixthly, the difference between of this embodiment and is that the top electrode layer is an ito layer, an oxyfluoride-doped sn layer or a metal layer, the metal is ag, au or pt, and the other steps are the same as those of to five.
A seventh embodiment mode, which is different from of the sixth embodiment modes in that the bottom electrode layer has a thickness of 2nm to 600nm and a resistance of 1 Ω to 10000 Ω, the electrochromic layer has a thickness of 10nm to 800nm, the complementary electrochromic layer has a thickness of 10nm to 800nm, the top electrode layer has a thickness of 2nm to 600nm and a resistance of 1 Ω to 10000 Ω, and other steps are the same as those of the seventh embodiment modes to sixteenth embodiment modes.
The preparation method of the fast-response all-solid-state electrochromic devices in the embodiment is completed according to the following steps:
, which adopts the following four methods to prepare the fast response all-solid-state electrochromic device:
method comprises sequentially depositing a bottom electrode layer, an electrochromic layer, a complementary electrochromic layer, a lithium layer and a top electrode layer on a substrate by vacuum coating, magnetron sputtering, vacuum thermal evaporation or electron beam evaporation;
the second method comprises the following steps: sequentially depositing a bottom electrode layer, an electrochromic layer, a lithium layer, a complementary electrochromic layer and a top electrode layer on a substrate by adopting a vacuum coating method, a magnetron sputtering method, a vacuum thermal evaporation method or an electron beam evaporation method;
the third method comprises the following steps: sequentially depositing a bottom electrode layer, a complementary color changing layer, an electrochromic layer, a lithium layer and a top electrode layer on a substrate by adopting a vacuum coating method, a magnetron sputtering method, a vacuum thermal evaporation method or an electron beam evaporation method;
the method four comprises the following steps: and sequentially depositing a bottom electrode layer, a complementary color changing layer, a lithium layer, an electrochromic layer and a top electrode layer on the substrate by adopting a vacuum coating method, a magnetron sputtering method, a vacuum thermal evaporation method or an electron beam evaporation method.
The principle and advantages of the embodiment are as follows:
, the embodiment can obtain novel fast response all-solid-state electrochromic device structures, the structures comprise four layers of structures of a bottom electrode layer, an electrochromic layer, a complementary electrochromic layer and a top electrode layer, color-changing ions are introduced by directly sputtering or evaporating metal lithium, and lithium diffuses into the electrochromic layer and the complementary electrochromic layer in the preparation process and does not exist independently due to small lithium atom radius;
secondly, after the fast-response all-solid-state electrochromic devices prepared by the embodiment are prepared, the color can be changed by applying voltage, and the color change function can also be optimized by heat treatment, wherein the heat treatment is carried out in vacuum, atmospheric atmosphere or inert gas atmosphere;
third, in the fast-response all-solid-state electrochromic devices of this embodiment, an intermediate electrolyte layer or an ion conducting layer is not required for manufacturing, which can reduce the production cost, improve the manufacturing efficiency, and reduce the internal impedance of the device, so the performance of the device is better than that of an electrochromic device having an electrolyte layer or an ion conducting layer structure, and the response time is less than 5 seconds.
The present invention can obtain kinds of fast response all-solid electrochromic devices.
A ninth embodiment mode, which is different from of the seventh embodiment mode to the eighth embodiment mode, in that the deposition rate of the bottom electrode layer is 0.01nm/s to 100nm/s, the deposition rate of the top electrode layer is 0.01nm/s to 100nm/s, the deposition rate of the electrochromic layer is 0.01nm/s to 100nm/s, the deposition rate of the complementary electrochromic layer is 0.01nm/s to 100nm/s, the deposition rate of the lithium layer is 0.01nm/s to 100nm/s, and the deposition time of the lithium layer is 2min to 60min, and other steps are the same as those of the seventh embodiment mode to the eighth embodiment mode.
Tenth embodiment mode differs from those of embodiment modes to nine in that the substrate is a heat-resistant substrate, and the substrate is used for heat treatment of a fast-response all-solid-state electrochromic device, the heat treatment is performed in vacuum, an atmospheric atmosphere or an inert gas atmosphere, the heat treatment temperature is 10 ℃ to 600 ℃, the heat treatment time is 10min to 400min, the inert gas is argon or nitrogen, and other steps are the same as those of embodiment modes to nine.
The following examples were used to demonstrate the beneficial effects of the present invention:
embodiment , fast response all-solid-state electrochromic devices are composed of a substrate, a bottom electrode layer, an electrochromic layer, a complementary color layer, a lithium layer and a top electrode layer, wherein the bottom electrode layer, the electrochromic layer, the complementary color layer and the top electrode layer are sequentially arranged on the substrate from bottom to top, the lithium layer is distributed in the electrochromic layer and the complementary color layer, and the preparation method comprises the following steps:
, depositing indium tin oxide on the glass by a vacuum thermal evaporation method, wherein the thickness of the indium tin oxide is 200nm, the deposition rate is 0.8nm/s, and the resistance is 50 omega;
depositing tungsten oxide on the indium tin oxide by adopting a vacuum thermal evaporation method, wherein the thickness of the tungsten oxide is 450nm, the deposition rate is 2nm/s, and the tungsten-oxygen ratio of the tungsten oxide is 1: 2.8;
depositing nickel oxide on the tungsten oxide by adopting a vacuum thermal evaporation method, wherein the thickness of the nickel oxide is 250nm, and the deposition rate is 1 nm/s;
depositing metal lithium on the nickel oxide by adopting a vacuum thermal evaporation method, wherein the deposition rate of the metal lithium is 0.1nm/s, and the deposition time of the metal lithium is 10 min;
depositing indium tin oxide by a vacuum thermal evaporation method, wherein the thickness of the indium tin oxide is 200nm, the deposition rate is 0.8nm/s, and the resistance is 50 omega, so as to obtain the fast-response all-solid-state electrochromic device;
and sixthly, carrying out heat treatment on the fast-response all-solid-state electrochromic device in the atmosphere, wherein the heat treatment temperature is 300 ℃, and the heat treatment time is 120 min.
FIG. 1 is a cross-sectional SEM image of fast response all-solid-state electrochromic devices prepared in example ;
in FIG. 1, ITO is indium tin oxide and Glass is Glass, and as can be seen from FIG. 1, lithium diffuses into tungsten oxide and nickel oxide, and the lithium layer does not exist independently.
Fig. 2 is a graph of the response times of fast responding all-solid-state electrochromic devices prepared in example .
As can be seen from fig. 2, the response time of the fast-response all-solid-state electrochromic device prepared in example was 2.5s (coloration) and 2.2s (discoloration).
The second embodiment comprises fast-response all-solid-state electrochromic devices, which comprise a substrate, a bottom electrode layer, an electrochromic layer, a complementary color-changing layer, a lithium layer and a top electrode layer, wherein the bottom electrode layer, the electrochromic layer, the complementary color-changing layer and the top electrode layer are arranged on the substrate from bottom to top in sequence, the lithium layer is distributed in the electrochromic layer and the complementary color-changing layer, and the specific preparation method comprises the following steps:
, depositing indium tin oxide on the glass by a vacuum thermal evaporation method, wherein the thickness of the indium tin oxide is 150nm, the deposition rate is 1nm/s, and the resistance is 90 omega;
depositing tungsten oxide on the indium tin oxide by adopting a vacuum thermal evaporation method, wherein the thickness of the tungsten oxide is 300nm, the deposition rate is 2.5nm/s, and the tungsten-oxygen ratio of the tungsten oxide is 1: 2.89;
depositing vanadium oxide on the tungsten oxide by adopting a vacuum thermal evaporation method, wherein the thickness of the vanadium oxide is 300nm, and the deposition rate is 0.5 nm/s;
depositing metal lithium on the nickel oxide by adopting a vacuum thermal evaporation method, wherein the deposition rate of the metal lithium is 0.05nm/s, and the deposition time of the metal lithium is 20 min;
depositing indium tin oxide by a vacuum thermal evaporation method, wherein the thickness of the indium tin oxide is 150nm, the deposition rate is 1nm/s, and the resistance is 90 omega, so as to obtain the fast-response all-solid-state electrochromic device;
and sixthly, carrying out heat treatment on the fast-response all-solid-state electrochromic device in the atmosphere, wherein the heat treatment temperature is 350 ℃, and the heat treatment time is 120 min.
The response times of the fast-response all-solid-state electrochromic device prepared in example two were 4.5s (coloration) and 2.8s (discoloration).
The third embodiment comprises fast-response all-solid-state electrochromic devices, which comprise a substrate, a bottom electrode layer, an electrochromic layer, a complementary electrochromic layer, a lithium layer and a top electrode layer, wherein the bottom electrode layer, the complementary electrochromic layer, the electrochromic layer and the top electrode layer are sequentially arranged on the substrate from bottom to top, the lithium layer is distributed in the electrochromic layer and the complementary electrochromic layer, and the specific preparation method comprises the following steps:
, depositing indium tin oxide on the glass by a vacuum thermal evaporation method, wherein the thickness of the indium tin oxide is 180nm, the deposition rate is 1.5nm/s, and the resistance is 60 omega;
depositing tungsten-doped nickel oxide on the indium tin oxide by adopting a vacuum thermal evaporation method, wherein the doping amount of tungsten in the tungsten-doped nickel oxide is 50%, the thickness of the tungsten-doped nickel oxide is 300nm, and the deposition rate is 1 nm/s;
depositing tungsten oxide on the tungsten-doped nickel oxide by adopting a vacuum thermal evaporation method, wherein the thickness of the tungsten oxide is 400nm, the deposition rate is 2.5nm/s, and the tungsten-oxygen ratio of the tungsten oxide is 1: 2.7;
depositing lithium metal on the tungsten oxide by adopting a vacuum thermal evaporation method, wherein the deposition rate of the lithium metal is 0.05nm/s, and the deposition time is 25 min;
depositing indium tin oxide by a vacuum thermal evaporation method, wherein the thickness of the indium tin oxide is 180nm, the deposition rate is 1.5nm/s, and the resistance is 60 omega, so as to obtain the fast-response all-solid-state electrochromic device;
and sixthly, carrying out heat treatment on the fast-response all-solid-state electrochromic device in the atmosphere, wherein the heat treatment temperature is 300 ℃, and the heat treatment time is 100 min.
The response times of the fast-response all-solid-state electrochromic device prepared in example three were 4.0s (coloration) and 1.9s (discoloration).
Claims (10)
- The fast-response all-solid-state electrochromic device is characterized in that fast-response all-solid-state electrochromic devices comprise a substrate, a bottom electrode layer, an electrochromic layer, a complementary color-changing layer, a lithium layer and a top electrode layer, wherein the bottom electrode layer, the electrochromic layer, the complementary color-changing layer and the top electrode layer are sequentially arranged on the substrate from bottom to top or the bottom electrode layer, the complementary color-changing layer, the electrochromic layer and the top electrode layer are sequentially arranged on the substrate from bottom to top, and the lithium layer is distributed in the electrochromic layer and the complementary color-changing layer.
- 2. The kinds of fast-response all-solid-state electrochromic devices according to claim 1, wherein the substrate is a heat-resistant substrate or a flexible substrate, the heat-resistant substrate is glass, and the flexible substrate is polyethylene terephthalate or polydimethylsiloxane.
- 3. The fast response all-solid-state electrochromic device according to claim 1, wherein the bottom electrode layer is an indium tin oxide layer, a fluorine-doped tin oxide layer or a metal layer, and the metal is silver, gold or platinum.
- 4. The kinds of fast-response all-solid-state electrochromic devices according to claim 1, wherein the electrochromic layer is a tungsten oxide layer or a vanadium oxide layer, and the tungsten oxide has a tungsten-to-oxygen ratio of 1 (1-3).
- 5. The kinds of fast-response all-solid-state electrochromic devices according to claim 1, wherein the complementary discoloration layers are a nickel oxide layer, a vanadium oxide layer, a tantalum oxide layer, a titanium oxide layer, a cobalt oxide layer, a zirconium oxide layer, an yttrium oxide layer and a nickel tungsten oxide layer, and the doping amount of tungsten in the nickel tungsten oxide layer is 1% -50%.
- 6. The fast response all-solid-state electrochromic device according to claim 1, wherein the top electrode layer is an indium tin oxide layer, a fluorine-doped tin oxide layer or a metal layer, and the metal is silver, gold or platinum.
- 7. The fast response all-solid-state electrochromic device according to claim 1, wherein the bottom electrode layer has a thickness of 2 nm-600 nm and a resistance of 1 Ω -10000 Ω, the electrochromic layer has a thickness of 10 nm-800 nm, the complementary electrochromic layer has a thickness of 10 nm-800 nm, and the top electrode layer has a thickness of 2 nm-600 nm and a resistance of 1 Ω -10000 Ω.
- 8. The method for preparing fast response all-solid-state electrochromic devices as claimed in any of claims 1 to 7, wherein the preparation method of fast response all-solid-state electrochromic devices is completed by the following steps:, which adopts the following four methods to prepare the fast response all-solid-state electrochromic device:method comprises sequentially depositing a bottom electrode layer, an electrochromic layer, a complementary electrochromic layer, a lithium layer and a top electrode layer on a substrate by vacuum coating, magnetron sputtering, vacuum thermal evaporation or electron beam evaporation;the second method comprises the following steps: sequentially depositing a bottom electrode layer, an electrochromic layer, a lithium layer, a complementary electrochromic layer and a top electrode layer on a substrate by adopting a vacuum coating method, a magnetron sputtering method, a vacuum thermal evaporation method or an electron beam evaporation method;the third method comprises the following steps: sequentially depositing a bottom electrode layer, a complementary color changing layer, an electrochromic layer, a lithium layer and a top electrode layer on a substrate by adopting a vacuum coating method, a magnetron sputtering method, a vacuum thermal evaporation method or an electron beam evaporation method;the method four comprises the following steps: and sequentially depositing a bottom electrode layer, a complementary color changing layer, a lithium layer, an electrochromic layer and a top electrode layer on the substrate by adopting a vacuum coating method, a magnetron sputtering method, a vacuum thermal evaporation method or an electron beam evaporation method.
- 9. The fast response all-solid-state electrochromic device preparation method according to claim 8, wherein the deposition rate of the bottom electrode layer is 0.01 nm/s-100 nm/s, the deposition rate of the top electrode layer is 0.01 nm/s-100 nm/s, the deposition rate of the electrochromic layer is 0.01 nm/s-100 nm/s, the deposition rate of the complementary electrochromic layer is 0.01 nm/s-100 nm/s, the deposition rate of the lithium layer is 0.01 nm/s-100 nm/s, and the deposition time of the lithium layer is 2 min-60 min.
- 10. The method of claim 8, wherein the substrate is a heat-resistant substrate, and the heat treatment is performed in vacuum, atmospheric atmosphere or inert gas atmosphere at a temperature of 10-600 deg.C for 10-400 min, wherein the inert gas is argon or nitrogen.
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| CN112764286A (en) * | 2021-01-29 | 2021-05-07 | 哈尔滨工业大学 | Thermal control device for intelligently regulating infrared emissivity and preparation method thereof |
| CN113204146A (en) * | 2021-05-07 | 2021-08-03 | 哈尔滨工业大学 | Repairable inorganic full-film electrochromic device taking water vapor as electrolyte and preparation method thereof |
| CN115469491A (en) * | 2022-08-04 | 2022-12-13 | 五邑大学 | Anti-dizziness rearview mirror and control method thereof |
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| CN113204146A (en) * | 2021-05-07 | 2021-08-03 | 哈尔滨工业大学 | Repairable inorganic full-film electrochromic device taking water vapor as electrolyte and preparation method thereof |
| CN113204146B (en) * | 2021-05-07 | 2023-04-25 | 哈尔滨工业大学 | Repairable inorganic full-film electrochromic device with water vapor as electrolyte and preparation method thereof |
| CN115469491A (en) * | 2022-08-04 | 2022-12-13 | 五邑大学 | Anti-dizziness rearview mirror and control method thereof |
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