CN108363256B - Electrochromic device and preparation method thereof - Google Patents
Electrochromic device and preparation method thereof Download PDFInfo
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- CN108363256B CN108363256B CN201810384944.1A CN201810384944A CN108363256B CN 108363256 B CN108363256 B CN 108363256B CN 201810384944 A CN201810384944 A CN 201810384944A CN 108363256 B CN108363256 B CN 108363256B
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- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1523—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material
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- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
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Abstract
The invention discloses an electrochromic device and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a tungsten oxide film precursor solution by using a sol-gel method, depositing the tungsten oxide film precursor solution on the surface of the first transparent conducting layer, and annealing to obtain a tungsten oxide electrochromic layer; preparing electrolyte by using a sol-gel method, and depositing the electrolyte on the surface of the tungsten oxide electrochromic layer to obtain an electrolyte layer; and bonding the electrolyte layer and the second transparent conductive layer, and drying and curing to obtain the electrochromic device. According to the technical scheme disclosed by the application, the tungsten oxide film precursor solution and the electrolyte are respectively prepared by using a sol-gel method and are deposited on the corresponding film layers to prepare the electrochromic device.
Description
Technical Field
The invention relates to the technical field of electronic devices, in particular to an electrochromic device and a preparation method thereof.
Background
Electrochromism refers to a phenomenon in which optical properties (reflectivity, transmittance, absorption, and the like) of a material undergo a stable and reversible color change under the action of an applied electric field, and is visually represented as a reversible change in color and transparency. Materials having electrochromic properties are referred to as electrochromic materials, and devices made with electrochromic materials are referred to as electrochromic devices.
The electrochromic device can be widely applied to buildings and vehicles, has adjustability of light absorption and transmission under the action of an electric field, can selectively absorb or reflect external heat radiation and internal heat diffusion, and reduces a large amount of energy which is consumed for office buildings and civil houses to keep cool in summer and warm in winter. Because about 53% of sunlight reaching the surface of the earth is near infrared light and the light has the function of regulating and controlling the temperature, the energy-saving purpose can be achieved by researching an electrochromic device with the function of regulating and controlling the transmittance of the near infrared light.
The electrochromic device taking tungsten oxide as the electrochromic layer has higher reflectivity to near infrared light after coloring, has softer color and better light-insulating performance, can achieve the heat-insulating effect similar to that of low-radiation glass, and is beneficial to reducing indoor energy consumption. At present, the tungsten oxide electrochromic layer and the electrolyte layer in the electrochromic device are often prepared by a magnetron sputtering method, CVD (Chemical Vapor Deposition method). However, these two preparation methods are complicated in process and expensive in equipment price.
In summary, how to simplify the manufacturing process of the electrochromic device and reduce the manufacturing cost of the electrochromic device is a technical problem to be solved urgently by those skilled in the art.
Disclosure of Invention
In view of this, an object of the present invention is to provide an electrochromic device and a method for manufacturing the same, so as to simplify a manufacturing process of the electrochromic device and reduce a manufacturing cost of the electrochromic device.
In order to achieve the above purpose, the invention provides the following technical scheme:
a preparation method of an electrochromic device comprises the following steps:
preparing a tungsten oxide film precursor solution by using a sol-gel method, depositing the tungsten oxide film precursor solution on the surface of the first transparent conducting layer, and annealing to obtain a tungsten oxide electrochromic layer;
preparing an electrolyte by using a sol-gel method, and depositing the electrolyte on the surface of the tungsten oxide electrochromic layer to obtain an electrolyte layer;
and bonding the electrolyte layer and the second transparent conducting layer, and drying and curing to obtain the electrochromic device.
Preferably, the annealing temperature is 250 ℃ and the annealing time is 2 h.
Preferably, the depositing the tungsten oxide film precursor solution on the surface of the first transparent conductive layer includes:
and spin-coating the tungsten oxide film precursor liquid to the surface of the first transparent conductive layer by using a spin-coating method.
Preferably, when the tungsten oxide film precursor solution is spin-coated on the surface of the first transparent conductive layer by using a spin coating method, the glue dripping speed is 1200r/min, the glue dripping time is 10s, the glue homogenizing speed is 3500r/min, and the glue homogenizing time is 25 s.
Preferably, when the tungsten oxide thin film precursor solution is spin-coated on the surface of the first transparent conductive layer by a spin coating method, the number of spin-coating times is 5.
An electrochromic device prepared by using the preparation method of any one of the electrochromic devices, the electrochromic device sequentially comprising: the device comprises a first transparent conducting layer, a tungsten oxide electrochromic layer, an electrolyte layer and a second transparent conducting layer.
Preferably, the tungsten oxide electrochromic layer is an amorphous tungsten oxide film.
Preferably, the thickness of the amorphous tungsten oxide thin film is 71 nm.
Preferably, the first transparent conductive layer and the second transparent conductive layer are made of ITO conductive glass.
Preferably, the first transparent conductive layer and the second transparent conductive layer are both FTO conductive glass.
The invention provides an electrochromic device and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a tungsten oxide film precursor solution by using a sol-gel method, depositing the tungsten oxide film precursor solution on the surface of the first transparent conducting layer, and annealing to obtain a tungsten oxide electrochromic layer; preparing electrolyte by using a sol-gel method, and depositing the electrolyte on the surface of the tungsten oxide electrochromic layer to obtain an electrolyte layer; and bonding the electrolyte layer and the second transparent conductive layer, and drying and curing to obtain the electrochromic device. According to the technical scheme disclosed by the application, the tungsten oxide film precursor solution and the electrolyte are respectively prepared by using a sol-gel method and are deposited on the corresponding film layers to prepare the electrochromic device.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a flowchart of a method for manufacturing an electrochromic device according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of an electrochromic device according to an embodiment of the present invention;
FIG. 3 is a graph showing transmittance curves of an electrochromic device in a colored state and a faded state in the visible-near infrared region according to an embodiment of the present invention;
FIG. 4 is a graph showing the distribution of the current peaks in the colored state and the bleached state of an electrochromic device obtained by scanning with an excitation voltage for 100cycles according to an embodiment of the present invention;
fig. 5 is a graph of current versus time for an electrochromic device scanned with an excitation voltage according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a flowchart of a method for manufacturing an electrochromic device according to an embodiment of the present invention is shown, where the method includes:
s11: and preparing a tungsten oxide film precursor solution by using a sol-gel method, depositing the tungsten oxide film precursor solution on the surface of the first transparent conducting layer, and annealing to obtain the tungsten oxide electrochromic layer.
The principle of the sol-gel method is that a compound containing high chemical activity components is used as a precursor, the raw materials are uniformly mixed in a liquid phase, hydrolysis and condensation chemical reactions are carried out, a stable transparent sol system is formed in a solution, sol is aged, and gel particles are slowly polymerized to form gel with a three-dimensional space grid structure, and a solvent losing fluidity is filled among gel grids to form gel.
The specific process for preparing the tungsten oxide film precursor solution by using the sol-gel method can be as follows: the required amount of the metal tungsten powder and the hydrogen peroxide is calculated in advance, and the required amount of the metal tungsten powder is added into the hydrogen peroxide. After the reaction was complete, glacial acetic acid and absolute ethanol were slowly added to form tungstic peroxy acid. Stirring the mixed solution after the mixing reaction at room temperature for 2h, then standing at room temperature for 70h, and then filtering the mixed solution for a plurality of times, generally 3 times, to finally obtain light yellow sol, namely to obtain the tungsten oxide film precursor solution. The preparation of the tungsten oxide film precursor liquid by using the sol-gel method can be realized without using complex and expensive equipment, and the technological process for preparing the tungsten oxide film precursor liquid by using the method is simpler.
In addition, when preparing a solution, the concentration of the solution can be controlled by controlling the amount of each component.
After the tungsten oxide film precursor solution is prepared, the tungsten oxide film precursor solution can be uniformly deposited on the surface of the first transparent conductive layer. After deposition, the first transparent conductive layer may be placed in a drying oven for drying, where the drying temperature may be set to 60 ℃ and the drying time may be set to 30min, so as to obtain the tungsten oxide electrochromic layer.
Before depositing the tungsten oxide film precursor solution on the first transparent conductive layer, the first transparent conductive layer needs to be cleaned and dried, and the cleaning and drying process may specifically be: by using a secondUltrasonically cleaning the first transparent conductive layer with alcohol, acetone and distilled water respectively, and using N2The first transparent conductive layer is dried by blowing to obtain a clean and dry first transparent conductive layer, so that the influence on the performance of the electrochromic device is reduced.
S12: and preparing an electrolyte by using a sol-gel method, and depositing the electrolyte on the surface of the tungsten oxide electrochromic layer to obtain the electrolyte layer.
Similarly, a sol-gel process can be used to prepare an electrolyte consisting of a polymer, a lithium salt or ionic liquid, and a plasticizer. Specifically, tetraethyl silicate can be used as a polymer, lithium acetate can be used as a lithium salt, and ethanol can be used as a plasticizer, and the reaction temperature and the proportion of each component are controlled to form the high polymer mixed electrolyte easy to charge transport. The preparation process specifically comprises the following steps: CA (Citric Acid ) was added to absolute ethanol and stirred at room temperature until dissolved. Then, tetraethyl silicate and lithium acetate are added to make the molar ratio of Si to CA 1:2, ethylene glycol is added, the temperature is raised to 60 ℃, and the mixture is stirred for 1 hour to obtain the required mixed polymer.
And uniformly depositing the obtained electrolyte on the surface of the tungsten oxide electrochromic layer to obtain an electrolyte layer. The electrolyte layer is an ion conductive layer, and generally refers to a polymer electrolyte, and the most representative polymer electrolyte matrix materials include polyether, polyacrylonitrile, polyvinylidene fluoride, and polymethacrylate, in which the polyether is mainly PEO (polyethylene oxide).
S13: and bonding the electrolyte layer and the second transparent conductive layer, and drying and curing to obtain the electrochromic device.
And (3) bonding the obtained electrolyte layer with the cleaned and dried second transparent conductive layer, and then drying and curing to prepare the electrochromic device, wherein the drying temperature is generally 60 ℃, and the curing time is generally 24 h.
It should be noted that the manner of cleaning and drying the second transparent conductive layer is the same as the manner of cleaning and drying the first transparent conductive layer, and details are not repeated here.
According to the technical scheme disclosed by the application, the tungsten oxide film precursor solution and the electrolyte are respectively prepared by using a sol-gel method and are deposited on the corresponding film layers to prepare the electrochromic device.
According to the preparation method of the electrochromic device, provided by the embodiment of the invention, the annealing temperature can be 250 ℃, and the annealing time can be 2 hours.
When the tungsten oxide film precursor solution is deposited on the first transparent conductive layer and annealed, the crystalline state of the tungsten oxide film can be controlled by controlling the annealing temperature. Experiments show that when the annealing temperature is 250 ℃ and the annealing time is 2 hours, the amorphous tungsten oxide film is obtained. The reaction time of the amorphous tungsten oxide in the coloring state and the fading state in the corresponding electrochromic device is short, the electrochromic efficiency is high, and specific parameters of the electrochromic device can refer to specific values obtained in the subsequent test of the electrochromic device.
In the preparation method of the electrochromic device provided by the embodiment of the invention, the depositing of the tungsten oxide film precursor solution on the surface of the first transparent conductive layer may include:
and spin-coating the tungsten oxide film precursor solution to the surface of the first transparent conductive layer by using a spin-coating method.
The prepared tungsten oxide film precursor liquid can be spin-coated on the surface of the first transparent conducting layer by using a spin-coating method, an electrochromic layer with higher density can be prepared by applying the spin-coating method to the preparation of an electrochromic device, and the obtained electrochromic layer is uniform in film thickness and beneficial to improving the performance of the electrochromic device.
Of course, the prepared tungsten oxide film precursor solution may be deposited on the surface of the first transparent conductive layer by dipping, spraying, and the like, and these specific deposition methods are all within the protection scope of the present invention, and the electrolyte may be deposited on the surface of the electrochromic layer by spin coating, dipping, spraying, and the like to obtain the electrolyte layer.
According to the preparation method of the electrochromic device, when the tungsten oxide film precursor liquid is spin-coated on the surface of the first transparent conductive layer by using a spin coating method, the glue dripping speed can be 1200r/min, the glue dripping time can be 10s, the glue homogenizing speed can be 3500r/min, and the glue homogenizing time can be 25 s.
When the tungsten oxide film precursor liquid is spin-coated on the surface of the first transparent conductive layer by using a spin coating method, the glue dripping speed can be 1200r/min, and the glue dripping time can be 10s, so that the tungsten oxide film precursor liquid can be better uniformly distributed on the surface of the first transparent conductive layer. After the tungsten oxide film precursor is dropped on the first transparent conductive layer, in order to better swing away the excess solution to obtain a tungsten oxide film with a relatively uniform film thickness, the spin coating rate may be 3500r/min, and the spin coating time may be 25 s.
According to the preparation method of the electrochromic device, provided by the embodiment of the invention, when the tungsten oxide film precursor solution is spin-coated on the surface of the first transparent conductive layer by using a spin coating method, the spin coating times are 5 times.
When the tungsten oxide film is prepared under the parameters, when the spin coating times are 5 times, that is, the electrochromic layer is composed of 5 layers of amorphous tungsten oxide films, the thickness of the corresponding amorphous tungsten oxide film is relatively proper, the performance of the corresponding electrochromic device is superior to that of the electrochromic device obtained under other spin coating times, and the performance parameters of the electrochromic device can also refer to specific values obtained by subsequent tests.
An embodiment of the present invention further provides an electrochromic device, which is prepared by using any one of the above electrochromic device preparation methods, and please refer to fig. 2, which shows a schematic structural diagram of an electrochromic device provided in an embodiment of the present invention, and the electrochromic device may sequentially include: a first transparent conductive layer 1, a tungsten oxide electrochromic layer 2, an electrolyte layer 3, and a second transparent conductive layer 4.
In the electrochromic device provided by the embodiment of the invention, the tungsten oxide electrochromic layer 2 is an amorphous tungsten oxide film.
When the annealing temperature is 250 ℃ and the annealing time is 2 hours, the obtained tungsten oxide electrochromic layer 2 is an amorphous tungsten oxide film, and when the tungsten oxide electrochromic layer is applied to an electrochromic device, the regulating and controlling capability of the obtained electrochromic device in a near-infrared light area is good, so that the indoor energy consumption can be greatly reduced, and the purpose of saving energy is achieved.
According to the electrochromic device provided by the embodiment of the invention, the thickness of the amorphous tungsten oxide film is 71 nm.
When the tungsten oxide film precursor solution is spin-coated by utilizing the spin coating parameters in the preparation method of the electrochromic device, the thickness of the amorphous tungsten oxide film obtained every time is constant. When the number of spin coating times is 5, the thickness of the obtained amorphous tungsten oxide film is 71nm, the reaction time of the corresponding tungsten oxide in a colored state and a faded state is short, the electrochromic efficiency is high, and the stability is good.
According to the electrochromic device provided by the embodiment of the invention, both the first transparent conducting layer 1 and the second transparent conducting layer 4 can be ITO conducting glass.
ITO conductive glass (i.e., tin-doped indium oxide conductive glass) having high transmittance, high conductivity, and high transmissivity can be used as the first transparent conductive layer 1 and the second transparent conductive layer 4 of the electrochromic device.
According to the electrochromic device provided by the embodiment of the invention, both the first transparent conducting layer 1 and the second transparent conducting layer 4 can be FTO (fluorine-doped tin oxide) conducting glass.
In addition to using ITO conductive glass as the first transparent conductive layer 1 and the second transparent conductive layer 4 of the electrochromic device, FTO conductive glass (i.e., fluorine-doped tin oxide conductive glass) having low resistivity, stable chemical properties, and relatively strong acid-base resistance at room temperature may be used as the first transparent conductive layer 1 and the second transparent conductive layer 4 of the electrochromic device.
Of course, aluminum-doped zinc oxide conductive glass or the like may also be used as the first transparent conductive layer 1 and the second transparent conductive layer 4 of the electrochromic device.
For specific description of relevant parts in the electrochromic device provided in the embodiment of the present invention, reference may be made to the above detailed description of corresponding parts in the preparation method of the electrochromic device provided in the embodiment of the present invention, and details are not repeated herein.
In order to describe the performance of the electrochromic device corresponding to the case where the annealing temperature is 250 ℃, that is, the electrochromic layer is an amorphous tungsten oxide film, and the number of layers of the amorphous tungsten oxide film is 5, a system assembled by a 2400 semiconductor parameter analyzer and an ultraviolet-visible spectrophotometer may be used to test the coloring/discoloring time, transmittance, electrochromic efficiency, and other performances of the electrochromic device in the visible light region and the near infrared light region under the action of different excitation voltages, and specifically, refer to fig. 3 to 5.
Fig. 3 is a graph of Transmittance of an electrochromic device in a Colored state and a Bleached state in a visible-near infrared region, where the abscissa represents a Wavelength (Wavelength), the ordinate represents Transmittance (transmission), and Δ T represents a difference in Transmittance between the Colored state (Colored state) and the Bleached state (blanketed state) at a current Wavelength. As can be seen from the figure, at a wavelength of 900nm, the transmittance corresponding to the colored state is 62.2%, the coloring time is 15.8s, the transmittance corresponding to the discolored state is 83%, and the discoloring time is 2.5s, and the discoloring time of the amorphous tungsten oxide film in the electrochromic device is shorter than the discoloring time (usually 20s) of the amorphous tungsten oxide film in the conventional electrochromic device, that is, the reaction time of the electrochromic device according to the present invention is relatively fast.
CE (Coloration Efficiency, electrochromic Efficiency) calculation formula:
CE＝ΔOD/ΔQ
ΔOD＝log(Tb/Tc)
wherein, TbTransmittance, T, corresponding to a faded statecIn the transmittance corresponding to the colored state, Δ OD represents the change in optical density of the electrochromic device in the colored state and the bleached state, and Δ Q represents the amount of charge injected/extracted per unit area during coloring/bleaching. Measuring Δ OD, and comparing Δ OD and TbAnd TcSubstituting into the above formula to obtain a CE of 78.8cm at 900nm wavelength2The CE of an electrochromic device prepared by the existing amorphous tungsten oxide film is 40-50cm under the wavelength of 900nm2The electrochromic efficiency of the electrochromic device prepared by the method is higher.
Fig. 4 is a Current peak distribution diagram of a colored state and a faded state of an electrochromic device obtained by scanning with an excitation voltage for 100 times in cycles according to an embodiment of the present invention, where the abscissa is Time (Time) and the ordinate is Current (Current). The excitation pulse with a scan amplitude of +2.5V, -2.5V and a scan time of 30s is used to scan 100cycles (100cycles), wherein +2.5V corresponds to the bleaching voltage and-2.5V corresponds to the colouring voltage. During scanning, the first transparent conducting layer and the second transparent conducting layer are respectively used as a positive electrode and a negative electrode, namely, the first transparent conducting layer and the second transparent conducting layer are tested only through excitation voltages with opposite polarities, so that the complexity of a peripheral circuit can be reduced, and the power consumption of an electrochromic device can be reduced. It can be seen from the figure that the electrochromic device shows the transition process between the colored state and the faded state each time when the electrochromic device is continuously scanned for 100 times in cycles, and the current peaks of the colored state and the faded state are very stable, which indicates that the electrochromic device has stable electrochromic performance and good fatigue resistance when the electrochromic device is operated in cycles under the condition.
Fig. 5 is a graph of current versus time for an electrochromic device scanned with an excitation voltage according to an embodiment of the present invention. As can be seen from the current value changes corresponding to the first ten periods and the last ten periods in the measurement process in the Coloring process (Coloring) when the voltage is-2.5V and the current value changes corresponding to the first ten periods and the last ten periods in the measurement process in the discoloring process (Bleaching) when the voltage is 2.5V in the figure, the amount of electric charges injected and extracted in the Coloring and discoloring processes of the electrochromic device is consistent when the electrochromic device is cycled for 100 times, and the electrochromic device has good invertibility and good stability.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Furthermore, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include elements inherent in the list. The term "comprising", without further limitation, means that the element so defined is not excluded from the group consisting of additional identical elements in the process, method, article, or apparatus that comprises the element. In addition, parts of the above technical solutions provided in the embodiments of the present invention that are consistent with the implementation principles of the corresponding technical solutions in the prior art are not described in detail, so as to avoid redundant description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. A preparation method of an electrochromic device is characterized by comprising the following steps:
preparing a tungsten oxide film precursor solution by using a sol-gel method, depositing the tungsten oxide film precursor solution on the surface of the first transparent conducting layer, and annealing to obtain a tungsten oxide electrochromic layer;
preparing an electrolyte by using a sol-gel method, and depositing the electrolyte on the surface of the tungsten oxide electrochromic layer to obtain an electrolyte layer;
bonding the electrolyte layer with the second transparent conductive layer, and drying and curing to obtain an electrochromic device;
the specific process for preparing the tungsten oxide film precursor solution by using the sol-gel method comprises the following steps: the method comprises the steps of calculating the required amount of metal tungsten powder and hydrogen peroxide in advance, adding the required amount of metal tungsten powder into the hydrogen peroxide, adding glacial acetic acid and absolute ethyl alcohol after the reaction is completed to form tungsten peroxy acid, stirring the mixed solution after the mixed reaction at room temperature for 2 hours, standing at room temperature for 70 hours, and filtering for several times to obtain a tungsten oxide film precursor solution;
the specific process for preparing the electrolyte by using the sol-gel method comprises the following steps: adding CA into absolute ethyl alcohol, stirring at room temperature until the CA is dissolved, then adding tetraethyl silicate and lithium acetate to enable the molar ratio of Si to CA to be 1:2, adding ethylene glycol, heating to 60 ℃, and stirring for 1h to obtain the required mixed polymer;
the annealing temperature is 250 ℃, and the annealing time is 2 hours;
depositing the tungsten oxide film precursor solution on the surface of the first transparent conducting layer, and the method comprises the following steps:
spin-coating the tungsten oxide film precursor liquid to the surface of the first transparent conductive layer by using a spin-coating method;
when the tungsten oxide film precursor liquid is spin-coated on the surface of the first transparent conductive layer by using a spin-coating method, the glue dripping speed is 1200r/min, the glue dripping time is 10s, the glue homogenizing speed is 3500r/min, the glue homogenizing time is 25s, and the spin-coating times are 5 times;
the tungsten oxide electrochromic layer is an amorphous tungsten oxide film, and the thickness of the amorphous tungsten oxide film is 71 nm.
2. An electrochromic device, characterized in that the electrochromic device is prepared by the electrochromic device preparation method of claim 1, and the electrochromic device sequentially comprises: the photoelectric composite film comprises a first transparent conducting layer, a tungsten oxide electrochromic layer, an electrolyte layer and a second transparent conducting layer, wherein the tungsten oxide electrochromic layer is an amorphous tungsten oxide film, and the thickness of the amorphous tungsten oxide film is 71 nm.
3. The electrochromic device according to claim 2, wherein the first and second transparent conductive layers are each ITO conductive glass.
4. The electrochromic device according to claim 2, wherein the first and second transparent conductive layers are both FTO conductive glass.
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| CN109581776B (en) * | 2019-01-02 | 2020-06-19 | 华南理工大学 | Low-cost electrochromic device and preparation method thereof |
| CN110204217A (en) * | 2019-04-11 | 2019-09-06 | 广东工业大学 | A kind of electrochromic device and preparation method thereof |
| CN110357454B (en) * | 2019-06-25 | 2022-01-21 | 嘉兴快闪新材料有限公司 | Drying method for reducing color fading of electrochromic film before annealing |
| CN111240119A (en) * | 2020-03-03 | 2020-06-05 | 中国科学院长春光学精密机械与物理研究所 | Electrochromic non-metal salt electrolyte composite material, preparation method and application |
| CN112327555A (en) * | 2020-11-20 | 2021-02-05 | 浙江工业大学 | Electrochromic device, preparation method thereof and application of electrochromic device in intelligent window |
| 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 |
| CN113359361B (en) * | 2021-05-08 | 2022-10-25 | 华南理工大学 | Microcavity-injected electrochromic device and preparation method and application thereof |
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| CN1928685A (en) * | 2006-09-28 | 2007-03-14 | 同济大学 | Method for preparing full solid electrochromic device with sol-gel |
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