CN115629501A - In-situ self-assembly large-area multicolor electrochromic device and preparation method and application thereof - Google Patents
In-situ self-assembly large-area multicolor electrochromic device and preparation method and application thereof Download PDFInfo
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- G—PHYSICS
- G02—OPTICS
- 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
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- G—PHYSICS
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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
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Abstract
The invention discloses an in-situ self-assembly large-area multicolor electrochromic device, a preparation method and application thereof, and relates to the technical field of electrochromic material modification. The method breaks through the technical bottleneck of the traditional electrochromic film and intelligent window preparation process, further improves the optical modulation delta T value (more than 70 percent and as high as 81.6 percent), has the advantages of economical preparation raw materials, simple and convenient operation, low requirement on equipment, high preparation efficiency, easy secondary recovery and treatment of waste liquid, economy, environmental protection and the like, is easy to popularize industrial production, and improves the market share and competitive advantage of the intelligent window field in future intelligent life.
Description
Technical Field
The invention relates to the technical field of electrochromic material modification, in particular to an in-situ self-assembled large-area multicolor electrochromic device and a preparation method and application thereof.
Background
Electrochromic is a phenomenon in which a material can reversibly switch its optical properties by applying an external potential/electric field, and reversibly insert/detach an electrochromic material layer by ions, so that the optical properties (transmittance, absorptance, reflectance) of a device are reversibly and stably changed, and the appearance of the device is represented by changes in color and transparency. At present, the electrochromic technology is widely applied to the fields of electrochromic intelligent windows, displays, aircraft portholes, stealth camouflage and the like.
As the demand for electrochromic smart windows has increased, the performance and demand for materials/devices has increased. In various traditional processes for preparing electrochromic thin film materials in the field, large-area production technology has great problems and challenges. Traditional preparation methods, such as an electrodeposition method (low yield due to nonuniform electric field distribution caused by resistance), a hydrothermal method (which requires high pressure and high temperature and is difficult to meet containers and equipment), a magnetron sputtering method (which requires high equipment cost and high production raw materials and power consumption under high vacuum conditions), are difficult to rapidly, efficiently, economically and environmentally produce large-area electrochromic films and intelligent windows in batches, and seriously hinder the industrial development and market popularization of electrochromic intelligent windows.
In order to further solve the problem of large-area production, patent application publication No. CN108828868a discloses a method for preparing an electrochromic film, wherein the prepared electrochromic film is formed by compounding a metal oxide, a Transparent Conductive Oxide (TCO) and a transparent conductive substrate. The technology adopts a blending method to prepare coating liquid of metal oxide and TCO, and then adopts a wet coating method to prepare the electrochromic oxide nano film. The advantages are that: the preparation method of the film is simple and convenient, and is suitable for large-scale production. The electrochromic film has the characteristics of short coloring and fading time, large optical modulation range, good cycle performance and low cost, and is suitable for manufacturing large-area electrochromic films. However, the optical modulation Δ T is not more than 70%, and the color development is not sufficiently noticeable. Compared with other electrochromic materials with excellent optical modulation range, the electrochromic material has the disadvantages of being large in size and difficult to improve the market share and competitive advantage of the intelligent window field in the future intelligent life.
Disclosure of Invention
The invention provides an in-situ self-assembly large-area multicolor electrochromic device and a preparation method and application thereof, so as to further improve the optical modulation delta T value.
In order to achieve the purpose, the invention provides the following technical scheme:
the utility model provides an in situ self-assembly large tracts of land polychrome electrochromic device, includes FTO/ITO/PET transparent conductive substrate and the thin film that discolours, the thin film that discolours comprises two-dimensional material film and electrochromic film, the two-dimensional material film is in through a mode in dripping, coating, spraying, spin-coating, blade coating, the printing by the two-dimensional material dispersion the FTO/ITO/PET transparent conductive substrate forms, electrochromic film is in through soaking, infiltration, spraying, spin-coating, drip coating, blade coating, a mode in the printing by electrochromic precursor solution two-dimensional material film surface forms.
Preferably, the two-dimensional material dispersion liquid is formed by dispersing a two-dimensional material into one of an acid solution, an alkali solution, an organic solvent and water and mixing, and the two-dimensional material is one or more of Mxene, graphene, graphite alkyne and black phosphorus; the electrochromic precursor solution is formed by dispersing an electrochromic precursor into one of an acid solution, an alkali solution, an organic solvent and water and mixing, wherein the electrochromic precursor is PB, polyaniline or WO 3 、TiO 2 、MoO 3 、Nb 2 O 5 、V 2 O 5 3,4-ethylenedioxythiophene.
Preferably, the preparation method of the two-dimensional material is one of a top-down mechanical stripping method, an intercalation stripping method, a direct ultrasonic stripping method, a shear stripping method and a selective etching method, or a bottom-up chemical synthesis method.
More preferably, the two-dimensional material dispersion liquid contains the two-dimensional material at a concentration of 1 to 50g/L.
More preferably, the concentration of the electrochromic precursor solution is 0.01-10 mol/L.
Preferably, the thickness of the two-dimensional material film is 20 nm-5 μm, the thickness of the electrochromic film is 100 nm-2 μm, and the time for attaching the electrochromic precursor solution is 1 min-24 h after the two-dimensional material film is preparedThe size of the prepared electrochromic film is 0.01-2 m 2 。
The preparation method of the in-situ self-assembled large-area multicolor electrochromic device comprises the following steps:
(1) Pretreating an FTO/ITO/PET transparent conductive substrate: cleaning, drying and ultraviolet ozone cleaning a transparent conductive substrate;
(2) Growing the electrochromic film: firstly, forming a two-dimensional material film on the transparent conductive substrate pretreated in the step (1) by using a two-dimensional material dispersion liquid, and then forming an electrochromic film on the two-dimensional material film by using an electrochromic precursor liquid.
Preferably, in the step (1), the transparent conductive substrate is ultrasonically cleaned in distilled water added with detergent, isopropanol added with NaOH, distilled water and absolute ethyl alcohol in sequence, and the ultrasonic cleaning time is 10-60 min each.
The application of the in-situ self-assembled large-area multicolor electrochromic device in the color-changing intelligent window.
The invention has the beneficial effects that:
the invention adopts a brand new two-dimensional material to assist in constructing a large-area electrochromic film material in situ, the electrochromic material and the two-dimensional conductive material are dispersed into one of acid solution, alkali solution and organic solvent to form coating liquid, and the coating liquid is further assembled to prepare the large-area electrochromic intelligent window. The method breaks through the technical bottleneck of the traditional electrochromic film and intelligent window preparation process, further improves the optical modulation delta T value (more than 70 percent and as high as 81.6 percent), has the advantages of economical preparation raw materials, simple and convenient operation, low requirement on equipment, high preparation efficiency, easy secondary recovery and treatment of waste liquid, economy, environmental protection and the like, is easy to popularize industrial production, and improves the market share and competitive advantage of the intelligent window field in future intelligent life. Meanwhile, the technology is expected to reform a brand-new preparation process in the electrochromic field, and the rapid development of the field is greatly promoted.
Drawings
FIG. 1 is a schematic representation of a large area multicolor electrochromic device (BP/PB film) prepared in example 1;
FIG. 2 is a graph of transmittance change curves of BP/PB thin film of large-area multi-color electrochromic device prepared in example 1 under different voltages;
FIG. 3 is a graph of the decay of the circulating current of 2000 loops of BP/PB film of the large-area multicolor electrochromic device prepared in example 1 (step voltage-0.8-0.6V);
FIG. 4 is a schematic representation of a large area multicolor electrochromic device (MXene/PB film) prepared in example 2;
FIG. 5 is a graph showing the transmittance change curves of MXene/PB film for large-area multicolor electrochromic devices prepared in example 2 under different voltages;
FIG. 6 is the decay curve diagram of the cycle current of 2000 loops of MXene/PB thin film of the large area multicolor electrochromic device prepared in example 2 (step voltage-0.8-0.6V);
FIG. 7 is a graph showing the transmittance and absorption of visible light and near infrared light at different voltages for devices fabricated at different temperatures;
FIG. 8 is a plot of cyclic voltammetry performed 100 times for devices fabricated at different temperatures;
fig. 9 is a graph of CV cyclic voltammetry tests performed on the same device at different voltages.
Detailed Description
The technical scheme of the invention is detailed in the following by combining the drawings and the embodiment.
Example 1
In this embodiment, the two-dimensional conductive material is black phosphorus, and the electrochromic material is a prussian blue analog, including pretreatment of conductive glass such as FTO/ITO/PET, preparation of a precursor solution, growth of an electrochromic film, and subsequent testing of the device. The specific operation is as follows:
1. ITO conductive glass pretreatment
And (3) carrying out ultrasonic cleaning on the ITO/FTO/PET glass in distilled water (added with detergent), isopropanol (added with NaOH), distilled water and absolute ethyl alcohol for 5-60 min, drying and carrying out ultraviolet ozone cleaning for 5-60 min to obtain the FTO conductive glass.
2. Precursor liquid preparation
1. Preparation of two-dimensional conductive material
Taking black phosphorus as an example: dissolving 3-300 mg BP into 3-300 mL NMP solvent, and mixing and stirring. And (3) carrying out ultrasonic treatment on the solution in an ice-water bath for 5-60 min, then carrying out ultrasonic treatment on the solution for 5-60 min by using a probe, and circulating for 1-10 periods. And then centrifuging the solution (the centrifugal speed is 100-8000 r/min, the centrifugal time is 5-60 min), taking out a larger product, and continuously centrifuging the rest solution (the centrifugal speed is 500-6000 r/min, the centrifugal time is 5-60 min) until a precipitate is generated. The precipitate was washed repeatedly with distilled water and ethanol. And adding the precipitate into ethanol to obtain black phosphorus dispersion liquid.
2. Precursor liquid preparation
Prussian blue and Prussian blue analogues are exemplified: 0.1-5 g of KCl and 0.1-5 g of FeCl 3 K of 0.1 to 5g 3 [Fe(CN) 6 ]Dissolving the solution into 10-500 mL of distilled water, dropwise adding 0.1-5 mL of concentrated hydrochloric acid, and stirring the solution until the solution is reddish brown clear solution to obtain a Prussian blue solution; mixing 0.1-5 g K 2 MoO 4 、0.1～5g K 3 [Fe(CN) 6 ]And 0.1-5 g of KCl are dissolved in 5-250 mL of distilled water, 0.1-5 mL of concentrated hydrochloric acid is dripped in the distilled water, the mixture is stirred to be a light yellow clear solution to obtain a MoOHCF Prussian blue analogue, and the two solutions are mixed according to a proportion to obtain a precursor solution.
3. Growing electrochromic film
And (3) uniformly dropwise adding the black phosphorus dispersion liquid in the step two onto the FTO glass in the step one, waiting for ethanol volatilization, and heating the FTO glass in a vacuum drying oven (the drying temperature is 25-80 ℃, and the drying time is 10-120 min). And (4) soaking the dried FTO into the precursor solution in the second step for 1 min-24 h. And soaking the FTO in distilled water for 1-60 min to prepare the electrochromic electrode shown in figure 1.
4. Assembly of large area electrochromic devices
And (3) assembling the large-area intelligent window: matching and assembling the ion storage layer with a proper size and the prepared electrochromic material film, and packaging the solid/liquid/gel electrolyte between the ion storage layer and the prepared electrochromic material film by adopting the processes of magnetron sputtering, thermal evaporation, blade coating, filling, curing and the like to prepare the large-area electrochromic intelligent window, wherein the substance of the large-area electrochromic intelligent window is shown in figure 1.
The electrochromic device is tested for different transmittances and absorptivities of visible light and near infrared waves under different voltages, the test results are respectively shown in fig. 2, and the optical modulation delta T% of the electrochromic device at the wavelength of 700nm is 81.6%; the fading time of the electrochromic film was 8.6s; as shown in fig. 3, after the cyclic processing of 2000 times, the film charge storage amount decreases by only 9.08%.
Example 2
In this embodiment, the two-dimensional conductive material is Mxene as an example, and the electrochromic material is prussian blue analog as an example, including FTO/ITO/PET conductive glass pretreatment, precursor solution preparation, electrochromic film growth, and subsequent testing of the device. The specific operation is as follows:
1. ITO conductive glass pretreatment
And (3) carrying out ultrasonic cleaning on the ITO/FTO/PET glass in distilled water (added with detergent), isopropanol (added with NaOH), distilled water and absolute ethyl alcohol for 30min, drying and carrying out ultraviolet ozone cleaning for 30min to obtain the FTO conductive glass.
2. Preparation of precursor solution
1. Preparation of two-dimensional conductive material
Taking Mxene as an example: weighing 0.1-1 g LiF by using balance, adding 10-30 mL of 3-12M HCl, stirring and reacting for 5-120 min, and weighing 0.1-2 g Ti by using balance 3 AlC 2 Adding the mixture into the reactor, adding 1-5 mL of HF by using a pipette, mixing and stirring the mixture for reaction, and etching the mixture (the temperature is 25-50 ℃ and the time is 12-48 h). And then centrifuging the solution (the centrifugal rotation speed is 2000-10000 r/min, the centrifugation time is 5-10 min), removing supernatant, adding a proper amount of deionized water, centrifuging again (the centrifugal rotation speed is 2000-10000 r/min, the centrifugation time is 5-10 min, the step is repeated for 2-5 times), adding a proper amount of ethanol into the centrifuge tube after the last centrifugation, shaking up, carrying out water bath ultrasonic treatment for 1.5-2 h, centrifuging again (the centrifugal rotation speed is 2000-10000 r/min, the centrifugation time is 5-10 min), and collecting the upper Mxene dispersion liquid.
2. Precursor liquid preparation
Prussian blue and Prussian blue analogues are exemplified: 0.1-5 g of KCl and 0.1-5 g of FeCl 3 K of 0.1 to 5g 3 [Fe(CN) 6 ]Dissolving the solution into 10-500 mL of distilled water, dropwise adding 0.1-5 mL of concentrated hydrochloric acid, and stirring the solution until the solution is reddish brown clear solution to obtain a Prussian blue solution; 0.1 to 5g K 2 MoO 4 、0.1～5g K 3 [Fe(CN) 6 ]And 0.1-5 g of KCl into 5-250 mL of distilled water, dropwise adding 0.1-5 mL of concentrated hydrochloric acid, and stirring to obtain a light yellow clear solution to obtain the MoOHCF Prussian blue analogue. And mixing the two solutions in proportion to obtain the precursor solution.
3. Electrochromic film growth
And (3) uniformly dropwise adding the Mxene dispersion liquid in the step two onto the FTO glass in the step one, waiting for ethanol volatilization, and heating the FTO glass in a vacuum drying oven (the drying temperature is 25-80 ℃, and the drying time is 10-120 min). And (4) soaking the dried FTO into the precursor solution in the second step for 1 min-24 h. And soaking the FTO in distilled water for 1-60 min to prepare the electrochromic electrode as shown in figure 2.
4. Assembly of large area electrochromic devices
The large-area intelligent window is assembled: matching and assembling the ion storage layer with a proper size and the prepared electrochromic material film, and packaging the solid/liquid/gel electrolyte between the ion storage layer and the prepared electrochromic material film by adopting the processes of magnetron sputtering, thermal evaporation, blade coating, filling, curing and the like to prepare the large-area electrochromic intelligent window, wherein the material object of the large-area electrochromic intelligent window is shown in figure 4.
The electrochromic device is tested for different transmittances and absorptivities of visible light and near infrared waves under different voltages, the test results are respectively shown in fig. 5, and the optical modulation delta T% of the electrochromic device at the wavelength of 700nm is 74%; the fading time of the electrochromic film was 10.6s; as shown in fig. 6, after the cyclic processing of 2000 times, the thin film charge storage amount decreases by only 7.78%.
Comparative tests were performed on electrochromic devices under different conditions. As shown in fig. 7, in the different transmittance and absorption rate tests of visible light and near-infrared wave under different voltages performed by the devices manufactured at different temperatures, the higher the temperature is within a certain temperature range, the larger the optical modulation rate Δ T% is; as shown in fig. 8, after the devices fabricated at different temperatures are subjected to cyclic voltammetry for 100 times, the higher the temperature is, the larger the charge storage amount is, the less the charge storage drop is; the CV cyclic voltammetry test is carried out on the same device under different voltages, the obtained result is shown in FIG. 9, the CV cyclic curves of the same device under different voltages show great difference, and when the negative voltage is lower than-1.0V and the positive voltage is higher than-2.4V, the CV curves have obvious polarization phenomenon. Comprehensively compares different voltage range cycles, and selects a cycle voltage range of-0.8-1.8V to be most suitable, and the voltage curves of different cycle CVs have higher coincidence and better stability.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (9)
1. The in-situ self-assembled large-area multicolor electrochromic device comprises an FTO/ITO/PET transparent conductive substrate and a color-changing film, and is characterized in that the color-changing film consists of a two-dimensional material film and an electrochromic film, the two-dimensional material film is formed on the FTO/ITO/PET transparent conductive substrate by one of dropping coating, spraying, spin coating, blade coating and printing of two-dimensional material dispersion liquid, and the electrochromic film is formed on the surface of the two-dimensional material film by one of soaking, infiltrating, spraying, spin coating, dropping coating, blade coating and printing of electrochromic precursor liquid.
2. The in-situ self-assembled large-area multicolor electrochromic device according to claim 1, wherein the two-dimensional material dispersion liquid is prepared by dispersing a two-dimensional material into one of an acid solution, an alkali solution, an organic solvent and water and mixing, and the two-dimensional material is one of Mxene, graphene, grapyne and black phosphorusOne or more kinds; the electrochromic precursor solution is formed by dispersing an electrochromic precursor into one of an acid solution, an alkali solution, an organic solvent and water and mixing, wherein the electrochromic precursor is PB, polyaniline or WO 3 、TiO 2 、MoO 3 、Nb 2 O 5 、V 2 O 5 3,4-ethylenedioxythiophene.
3. The in-situ self-assembled large-area multi-color electrochromic device according to claim 2, wherein the two-dimensional material is prepared by one of a top-down mechanical lift-off method, an intercalation lift-off method, a direct ultrasonic lift-off method, a shear lift-off method and a selective etching method, or a bottom-up chemical synthesis method.
4. The in-situ self-assembled large area multicolor electrochromic device according to claim 2, wherein the two-dimensional material dispersion contains the two-dimensional material at a concentration of 1 to 50g/L.
5. The in-situ self-assembled large area multicolor electrochromic device according to claim 2, wherein the concentration of the electrochromic precursor solution is 0.01-10 mol/L.
6. The in-situ self-assembled large-area multicolor electrochromic device according to claim 1, wherein the thickness of the two-dimensional material film is 20nm to 5 μm, the thickness of the electrochromic film is 100nm to 2 μm, the time for attaching the electrochromic precursor solution is 1min to 24h after the two-dimensional material film is prepared, and the size of the prepared electrochromic film is 0.01 to 2m 2 。
7. The method of any of claims 1 to 6 for the preparation of an in-situ self-assembled large area multicolor electrochromic device comprising the steps of:
(1) Pretreating the FTO/ITO/PET transparent conductive substrate: cleaning, drying and ultraviolet ozone cleaning a transparent conductive substrate;
(2) Growing the electrochromic film: firstly, forming a two-dimensional material film on the transparent conductive substrate pretreated in the step (1) by using a two-dimensional material dispersion liquid, and then forming an electrochromic film on the two-dimensional material film by using an electrochromic precursor liquid.
8. The method for preparing an in-situ self-assembled large-area multicolor electrochromic device according to claim 7, wherein in the step (1), the transparent conductive substrate is sequentially subjected to ultrasonic cleaning in distilled water added with detergent, isopropanol added with NaOH, distilled water and absolute ethyl alcohol, and each ultrasonic cleaning time is 10-60 min.
9. Use of an in-situ self-assembled large area multicolor electrochromic device according to any one of claims 1 to 6 in a color-shifting smart window.
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