CN111665673A - Electrochromic flexible display device with parallel structure and preparation method thereof - Google Patents
Electrochromic flexible display device with parallel structure and preparation method thereof Download PDFInfo
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Images
Classifications
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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
- G02F1/153—Constructional details
- G02F1/155—Electrodes
-
- 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
- G02F1/1506—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 caused by electrodeposition, e.g. electrolytic deposition of an inorganic material on or close to an electrode
- G02F1/1508—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 caused by electrodeposition, e.g. electrolytic deposition of an inorganic material on or close to an electrode using a solid electrolyte
-
- 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
- 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
- G02F1/1516—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 organic material
-
- 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
- G02F1/153—Constructional details
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- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention discloses an electrochromic flexible display device with a parallel structure, which sequentially comprises the following structures: the transparent conductive electrode, the electrochromic layer I, the electrochromic layer II and the electrolyte layer; the transparent conductive electrode is composed of a flexible substrate and a transparent conductive layer covered on the flexible substrate, the transparent conductive layer is composed of an area A and an area B, and the area A and the area B are separated by a spacing channel and are not communicated with each other; at least part of the area A is covered with an electrochromic layer, namely an electrochromic layer I; at least part of the area B is covered with an electrochromic layer, namely an electrochromic layer II; the spacing channel between the area A and the area B does not cover the electrochromic layer; the electrolyte layer at least covers the first electrochromic layer, the second electrochromic layer and the area between the first electrochromic layer and the second electrochromic layer. The electrochromic device obtained by the invention is ultrathin, flexible and foldable, and the colors of the color changing layers are not mutually interfered, so that the effect of multicolor display can be achieved.
Description
Technical Field
The invention relates to an electrochromic flexible display device with a parallel structure and a preparation method thereof.
Background
At present, most display devices such as displays, electronic paper, electronic advertising screens and the like in the market adopt liquid crystal or electrophoresis technology. The liquid crystal has large energy consumption, is not transparent and can not realize flexible display; electrophoresis can only display transparent and opaque or fixed colors in general, and the application field is single. The flexible display device based on the conductive polymer electrochromic material has huge market application value in the aspects of electronic paper, displays and the like due to the characteristics of flexibility, convenience in carrying, no view angle limit, energy conservation, power conservation and the like.
A typical electrochromic device is a sandwich structure, consisting of five layers: the transparent conductive electrode, the electrochromic layer, the ion conductive layer, the ion storage layer and the other transparent conductive electrode are sequentially arranged, wherein the common transparent conductive electrode is ITO or FTO glass. Conventional rigid structure electrochromic devices have met with significant success, with high cycling stability paving the way to commercialization, but the demand for flexible display devices is difficult to meet because the rigid substrates are brittle and do not bend easily. To solve this problem, recent work has reported replacing rigid substrates with flexible transparent substrates, the most popular of which is ethylene terephthalate (PET). PET is highly transparent and flexible, and a conductive layer (such as PEDOT: PSS or silver nanowire) is introduced on the surface of the PET, so that the conductive capability of the PET can be greatly improved, and the electrode still keeps good conductivity after being folded for many times.
On the basis, the invention provides a novel electrochromic device structure with a parallel structure, namely a flexible patterned electrode with high transmittance and high conductivity is prepared; further, the same or different polymer-based Electrochromic (EC) materials are prepared on the patterned electrode by a full solution process; finally, the flexible multicolor display device with the all-solid-state side-by-side structure is assembled. This device compares in traditional sandwich structure device: the original two electrodes are changed into the existing single-layer electrode, and the electrolyte layer and the electrochromic layer are arranged side by side, so that an ultrathin, flexible and foldable novel electrochromic device is expected to be obtained; and the colors of the color changing layers are not mutually interfered, so that the effect of multicolor display can be achieved. Therefore, the electrochromic flexible display device with the parallel structure, which is prepared by the invention, has great application potential in the application fields of flexibility and wearability.
Disclosure of Invention
The invention aims to combine the existing electrochromic technology with a mechanical flexible material, and provides an electrochromic flexible display device with a parallel structure and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
an electrochromic flexible display device having a side-by-side structure, the structure comprising in order: the transparent conductive electrode, the electrochromic layer I, the electrochromic layer II and the electrolyte layer; the transparent conductive electrode is composed of a flexible substrate and a transparent conductive layer covered on the flexible substrate, the transparent conductive layer is composed of an area A and an area B, and the area A and the area B are separated by a spacing channel and are not communicated with each other; at least part of the area A is covered with an electrochromic layer, namely an electrochromic layer I; at least part of the area B is covered with an electrochromic layer, namely an electrochromic layer II; the spacing channel between the area A and the area B does not cover the electrochromic layer; the electrolyte layer at least covers the first electrochromic layer, the second electrochromic layer and the area between the first electrochromic layer and the second electrochromic layer, so that the first electrochromic layer and the second electrochromic layer can carry out ion transmission under the condition of not directly contacting.
In the invention, the spacing channels can be equally spaced or unequally spaced, and can be linear or curved. In the specific embodiment of the invention, for convenience, the spacing channels are linear channels with equal spacing, namely square channels, and the transparent conducting layer is divided into a left-right symmetrical area A and an area B.
In the present invention, the first electrochromic layer may completely cover the region a of the transparent conductive layer, or may partially cover the region a of the transparent conductive layer, or the second electrochromic layer. Preferably, the first electrochromic layer and the second electrochromic layer are symmetrically distributed on two sides of the spacing channel.
In the present invention, the electrolyte layer functions to allow ion transport between the first electrochromic layer and the second electrochromic layer without direct contact. Thus, the electrolyte layer covers at least the first electrochromic layer and the second electrochromic layer and the area between them.
Preferably, part of the region A is only covered with the transparent conducting layer without covering the electrochromic layer and the electrolyte layer, and part of the region B is also only covered with the transparent conducting layer without covering the electrochromic layer and the electrolyte layer, and the two exposed transparent conducting layers can be directly connected with an external circuit. If the areas A and B are completely covered by the electrolyte layer, the conductive layer can be led to the outside by copper wires to be connected with an external circuit.
The present invention has no particular requirement on the selection of the flexible substrate, the transparent conductive layer, the electrochromic layer and the electrolyte layer, and the skilled person can select the flexible substrate, the transparent conductive layer, the electrochromic layer and the electrolyte layer according to actual conditions, for example, according to literature reports.
Specifically, the flexible substrate may be polybutylene terephthalate (PET), polyurethane, Polydimethylsiloxane (PDMS), or the like. The conductive material forming the transparent conductive layer may be indium tin oxide, fluorine-doped tin oxide, PEDOT: PSS, silver nanowires (AgNWs), or the like. The preparation of the transparent conducting layer and the spacing channel can be realized by introducing a mask plate.
The first electrochromic layer and the second electrochromic layer can be respectively and independently selected from PPRODOT, ProDOT-FI, ProDOT-Cbz, ProDOT-Py films and the like.
The electrolyte layer may be made of a solid polymer electrolyte based on the PMMA system or based on the PTMA system.
The invention particularly recommends that the electrochromic flexible display device with the parallel structure is prepared according to the following method:
(1) placing a mask plate with a certain shape on a transparent flexible substrate, uniformly spraying dispersion liquid containing conductive substances onto the transparent flexible substrate on which the mask plate is placed by using a spray gun to form a transparent conductive layer, controlling the shape of the mask plate to enable the transparent conductive layer to be composed of an area A and an area B, wherein the area A and the area B are separated by an interval channel and are not communicated with each other, and annealing to obtain a stable flexible patterned transparent conductive electrode;
(2) respectively spraying electrochromic polymers on the area A and the area B of the transparent conductive layer prepared in the step (1) by adopting a spraying method to form a first electrochromic layer and a second electrochromic layer, wherein the first electrochromic layer at least covers part of the area A, the second electrochromic layer at least covers part of the area B of the transparent conductive layer, and an interval channel between the area A and the area B is not sprayed with the electrochromic layer;
(3) and (3) coating a layer of gel electrolyte on the surface of the material obtained in the step (2) in a scraping mode, enabling the gel electrolyte layer to at least cover the first electrochromic layer, the second electrochromic layer and the area between the first electrochromic layer and the second electrochromic layer, drying the obtained device in an oven, and finally obtaining the electrochromic flexible display device with the parallel structure.
Further, in the step (1), the annealing temperature is 40-60 ℃, and the annealing time is 30-60 min.
Further, in the step (3), the drying temperature of the device is 40-70 ℃, and the drying time is 30-60 min.
In a specific embodiment of the present invention, the dispersion liquid containing a conductive substance is prepared by the following method: quickly adding dopamine hydrochloride and alginic acid into 25-28 wt% ammonia solution, wherein the mass ratio of the dopamine hydrochloride to the alginic acid is 1: 5-1: 4, stirring the mixture at room temperature to react to obtain a uniform dark mixed solution; then, adding absolute ethyl alcohol into the mixed solution to precipitate the compound, centrifuging the precipitate, and finally washing with ethyl alcohol and a small amount of water to obtain the Aa-PDA compound; adding AgNWs dispersion liquid and an Aa-PDA compound into a water/ethanol mixed solvent, wherein the mass ratio of the Aa-PDA compound to the AgNWs is 1: 7-1: and 10, carrying out ultrasonic dispersion to obtain a uniform dispersion liquid containing the conductive substance.
In the present invention, the AgNWs dispersion can be prepared from commercially available products or from the literature.
Further, the stirring reaction time is 12-24 h, and the volume ratio of the mixed solution to the absolute ethyl alcohol is 1: 2-1: 3.
further, the concentration of AgNWs in the dispersion liquid containing the conductive substance is 0.5-0.7 mg.L-1。
Further, in the water/ethanol mixed solvent, the volume ratio of ethanol to water is 2: 1-1: 4.
in a specific embodiment of the present invention, the electrochromic polymer is a conductive polymer PProDOT, and can be prepared by the following method: adding a catalyst p-toluenesulfonic acid into a mixture of 3, 4-dimethoxythiophene and dibromoneopentyl glycol dissolved in anhydrous toluene, refluxing the mixture for 6-12 hours, and extracting and passing through a column to obtain a product A; mixing the product A and 2-ethylhexanol, adding the mixture into DMF, adding NaH catalyst, fully reacting at a certain temperature, and extracting and passing through a column to obtain a product B; carrying out NBS bromination reaction on the product B to obtain a product C; mixing the product B and the product C in DMAc, and carrying out chemical polymerization to obtain a final soluble conductive polymer material PPRODOT; the reaction formula is shown as follows:
further, the amount ratio of the substances of 3, 4-dimethoxythiophene and dibromoneopentyl glycol in the mixture is 1: 1-1: 3, the reflux temperature is 110-130 ℃.
Further, the mass ratio of the product A to the 2-ethylhexanol is 1: 3-1: and 5, the reaction temperature is 70-100 ℃, and the reaction time is 3-4 h.
Further, the mass ratio of the product B to NBS is 1: 2-1: and 3, carrying out bromination reaction at room temperature for 12-24 hours.
Further, the ratio of the amount of the product B to the amount of the product C in the chemical combination polymerization process is 1: 1-1: 2, the reaction temperature of the chemical polymerization is 100-150 ℃, and the reaction time is 12-24 h.
In a specific embodiment of the present invention, the gel electrolyte is prepared by the following method: mixing a plasticizer and a polymer binder according to a mass ratio of 1: 2-1: 5, mixing, heating and swelling, and marking as a system a; adding a supporting electrolyte into a solvent, and carrying out ultrasonic treatment until the supporting electrolyte is completely dissolved, and marking as a system b; mixing the system a and the system b, wherein the mass ratio of the supporting electrolyte to the plasticizer is 1: 3-1: 4, performing ultrasonic treatment until the solution is uniform, and performing rotary evaporation on the obtained solution to remove part of the solvent to obtain a gel electrolyte; the mass ratio of the plasticizer to the polymer binder is as follows.
Further, the mass ratio of the supporting electrolyte to the solvent is 1: 5-1: 7.
further, the polymer binder is polymethyl methacrylate (PMMA), polyvinylidene fluoride, polyethylene oxide, polyvinylidene fluoride-hexafluoropropylene or polyacrylonitrile.
Further, the plasticizer is propylene carbonate, ethylene carbonate, dimethyl carbonate or diethyl carbonate.
Further, the supporting electrolyte is lithium perchlorate, lithium tetrafluoroborate, 1-butyl-3-methylimidazolium hexafluorophosphate, 1-butyl-3-methylimidazolium trifluoromethanesulfonate or 1-butyl-3-methylimidazolium bistrifluoromethylsulfonyl imide.
Further, the solvent is acetonitrile and/or dichloromethane.
Compared with the prior art, the invention has the following beneficial effects:
(1) compared with the traditional sandwich structure device, the electrochromic flexible display device with the parallel structure is designed in the invention: the original two electrodes are changed into the existing single-layer electrode, and the electrolyte layer and the electrochromic layer are arranged in parallel, so that the novel ultrathin, flexible and foldable electrochromic device is obtained; and the colors of the color-changing layers are not mutually interfered, so that the effect of multicolor display can be achieved, and the color-changing layer has potential application in the display fields of electronic paper, displays, intelligent watches and the like.
(2) The device can adopt a full-solution processing technology, the operation process is simple and convenient, the energy consumption is low, the raw material cost is low, and meanwhile, the preparation process of the device is safe and pollution-free, and meets the requirements of green production and the ecological concept of environmental protection.
Drawings
Fig. 1 is a schematic structural view of an electrochromic flexible display device in a side-by-side configuration; the transparent substrate comprises a transparent substrate 1, a transparent conducting layer 2, an electrolyte layer 3, an electrochromic layer I, an electrochromic layer II and an electrochromic layer I, and is characterized in that the transparent substrate is exposed, the transparent conducting layer 2 is transparent, the electrolyte layer 4 is transparent, and the electrochromic layer I, the electrochromic layer II and the electrochromic layer II are transparent.
FIG. 2 is a schematic structural diagram of a mask, where 6 is a space and 7 is a hollow portion.
FIG. 3 is a color change effect diagram of a device prepared in example 5.
FIG. 4 is a graph of absorbance at all wavelength bands of the device prepared in example 5 after scanning at 1100-300 nm.
FIG. 5 is a graph showing the optical contrast of the device prepared in example 5 at a wavelength of 545 nm.
Detailed Description
The invention is further described below by means of specific examples, without restricting its scope to these.
Some of the starting materials and reagents used in the present invention are commercially available.
Example 1: preparation of patterned flexible transparent conductive electrode
0.125g dopamine hydrochloride and 0.725g alginic acid were quickly added to the ammonia solution (50ml, 25-28 wt%) and the mixture was allowed to react for 12h with stirring at room temperature to obtain a homogeneous dark solution. Thereafter, 100mL of anhydrous ethanol was added to the solution to precipitate the complex, and the precipitate was centrifuged at 8000 rpm. Finally, the resulting complex was washed twice with ethanol and a small amount of water to obtain an Aa-PDA complex.
A dispersion of AgNWs in absolute ethanol (5 mg. mL)-1Purchased from cryolite nano technologies limited, suzhou) and Aa-PDA complexes were added to 100mL of a water/ethanol solvent mixture (volume ratio 1: 1) in and obtained by ultrasonic dispersionAnd (4) homogenizing the dispersion. Wherein the concentrations of AgNWs and Aa-PDA in the dispersion are 0.65 mg/mL-1And 0.08 mg. mL-1。
Then, a mask plate (shown in figure 2) with the overall size of 2cm × 2cm, the symmetrical hollow sizes of two spaced sides of 0.8cm × 2cm and the spaced size of 0.4cm × 2cm is placed in the middle of a clean and dry transparent PET flexible substrate, 2mL of dispersion liquid is uniformly sprayed on the mask plate by using a spray gun, the mask plate is taken off, a transparent conducting layer which is symmetrical left and right and is not communicated with each other is formed as shown in figure 1, the left part and the right part are respectively marked as an area A and an area B, the sizes of the area A and the area B are both 0.8cm × 2cm, annealing is carried out for 30min at the temperature of 50 ℃ to obtain a stable conducting electrode, and the resistance value of the sheet resistor is 7.5 omega · sq-1The transmittance was 80.16% (545 nm).
Example 2: preparation of electrochromic layer
To a round-bottomed flask containing 30mL of anhydrous toluene were added 1.89g of dibromoneopentyl glycol and 0.5g of p-toluenesulfonic acid, and 1.04g of 3, 4-dimethoxythiophene under a nitrogen atmosphere. After the mixed solution was warmed to 130 ℃, it was refluxed at a constant temperature for 12 hours. After the reaction is finished, extracting and passing through a column, and performing spin drying to obtain a white solid product A. Then, 1.05g of NaH is continuously weighed and added into the mixed solution of 2-ethyl hexanol and DMF, 1.5g of product is added after stirring for 1h, and the temperature is raised to 90 ℃ for reaction for 4 h. After the reaction is finished, the mixture is extracted and passed through a column, and is dried by spinning to obtain a colorless oily product B. And continuously weighing 1.0g of the product B, adding the product B into 30mL of trichloromethane, carrying out light shading reaction at normal temperature for 12h, and then extracting and passing through a column to obtain a product C. Mixing the product B and the product C, reacting at constant temperature of 120 ℃ for 24h to obtain the final mauve electrochromic conducting polymer D (PPRODOT).
Conducting Polymer D was dissolved in DCM to prepare 5 mg. multidot.mL-1The spraying liquid of (1) was continuously and uniformly sprayed in the region a and the region B of the transparent conductive layer prepared in example 1 while controlling the height of the spraying to be 15cm, to obtain a first electrochromic layer and a second electrochromic layer, which were bilaterally symmetric in the spacing channel, as shown in fig. 1, and were 0.8cm × 1cm in size, respectively, without spraying an electrochromic layer in the spacing channel.
Example 3: preparation of the electrolyte layer
Placing 2g of polymer binder PMMA and 8g of plasticizer PC in a 30ml reagent bottle, sealing the reagent bottle, and heating and swelling in a 75 ℃ oven for 20h, and marking as a system a; a mixture of 4g of acetonitrile and 10g of dichloromethane was taken and placed in a 30ml reagent bottle, and then 4g of supporting electrolyte LiBF was added4Adding the mixture into a mixed solvent, and carrying out ultrasonic treatment for 30min until the electrolyte is completely dissolved, and marking as a system b; and (3) mixing the system a and the system b, carrying out ultrasonic treatment on the obtained mixed system for 30min until the mixed system is uniform, and removing part of the solvent from the obtained solution through rotary evaporation to obtain the polymer gel electrolyte.
Example 4: preparation of electrochromic flexible display device with parallel structure
As shown in fig. 1, 1g of the gel-state electrolyte obtained in example 3 is uniformly applied to the surfaces of the first electrochromic layer and the second electrochromic layer prepared in example 2 and covers the gap region between the first electrochromic layer and the second electrochromic layer, at this time, the transparent conductive layers with partial areas in the region a and the region B are exposed (the two exposed transparent conductive layers can be directly connected with an external circuit in subsequent applications), and the obtained device is placed into an oven at 50 ℃ for drying for 30min, so that an electrochromic flexible display device with a parallel structure is finally obtained.
Example 5: spectroelectrochemistry and electrochromism performance test of electrochromic flexible display device with parallel structure
As shown in fig. 2, under a voltage of 1.0V, the positive electrode of the electrochromic flexible display device with the parallel structure prepared in example 4 is changed from purple red to a transparent state; when the voltage returns to-1.0V, the anode of the device returns to the purple state, and the cathode of the device changes to a transparent state.
And carrying out absorbance test of the whole wave band on the anode of the device, adopting a technology of combining an electrochemical workstation and an ultraviolet spectrometer, setting the electrochemical workstation to be a constant potential electrolysis method, setting the ultraviolet spectrum to be absorbance of the whole wave band, and setting the scanning range to be 1100-300 nm. As shown in FIG. 3, when a constant potential of 0V was applied, a significant absorption peak appeared at a wavelength of 545nm, and a significant change occurred with an increase in applied voltage. And with the increase of the applied voltage, a remarkable peak shape appears around 900nm, and the peak falls off remarkably when the applied voltage reaches 1.1V, which indicates that 1.0V is the optimum voltage that the electrochromic device can bear.
In order to detect the contrast of the electrochromic device, taking the device anode as an example, an electrochemical workstation and an ultraviolet spectrometer are used together, and the electrochemical workstation is set to be a multi-potential step method: setting ultraviolet spectrum as spectral dynamics and setting wavelength as 545 nm; the initial potential was-1.0V, the end potential was 1.0V, the potential pulse width was 30s, and the scanning time was 1000 s. The resulting data are shown in fig. 4. The optical contrast of the device at 545nm was 45.8%.
Claims (10)
1. An electrochromic flexible display device having a side-by-side structure, the structure comprising in order: the transparent conductive electrode, the electrochromic layer I, the electrochromic layer II and the electrolyte layer; the transparent conductive electrode is composed of a flexible substrate and a transparent conductive layer covered on the flexible substrate, the transparent conductive layer is composed of an area A and an area B, and the area A and the area B are separated by a spacing channel and are not communicated with each other; at least part of the area A is covered with an electrochromic layer, namely an electrochromic layer I; at least part of the area B is covered with an electrochromic layer, namely an electrochromic layer II; the spacing channel between the area A and the area B does not cover the electrochromic layer; the electrolyte layer at least covers the first electrochromic layer, the second electrochromic layer and the area between the first electrochromic layer and the second electrochromic layer, so that the first electrochromic layer and the second electrochromic layer can carry out ion transmission under the condition of not directly contacting.
2. An electrochromic flexible display device with a juxtaposed structure as claimed in claim 1, characterized in that: the spacing channels are linear channels with equal intervals, namely square channels, and divide the transparent conducting layer into a left area A and a right area B which are symmetrical.
3. An electrochromic flexible display device with a juxtaposed structure as claimed in claim 1 or 2, characterized in that: the first electrochromic layer and the second electrochromic layer are symmetrically distributed on two sides of the spacing channel.
4. An electrochromic flexible display device with a juxtaposed structure as claimed in any one of claims 1 to 3, characterized in that: the transparent conducting layer is only covered on one part of the area A without covering the electrochromic layer and the electrolyte layer, and the transparent conducting layer is only covered on one part of the area B without covering the electrochromic layer and the electrolyte layer, and the two exposed transparent conducting layers can be directly connected with an external circuit.
5. An electrochromic flexible display device with a juxtaposed structure as claimed in any one of claims 1 to 4, characterized in that: the flexible substrate is polybutylene terephthalate, polyurethane or polydimethylsiloxane; the conductive material forming the transparent conductive layer is indium tin oxide, fluorine-doped tin oxide, PEDOT PSS or silver nanowires.
6. An electrochromic flexible display device with a juxtaposed structure as claimed in any one of claims 1 to 4, characterized in that: the first electrochromic layer and the second electrochromic layer are respectively and independently selected from PPRODOT, ProDOT-FI, ProDOT-Cbz or ProDOT-Py films.
7. An electrochromic flexible display device with a juxtaposed structure as claimed in any one of claims 1 to 4, characterized in that: the electrolyte layer is made of a solid polymer electrolyte based on a PMMA system or a PTMA system.
8. A method of manufacturing an electrochromic flexible display device having a side-by-side structure as claimed in claim 1, which is performed according to the following steps:
(1) placing a mask plate with a certain shape on a transparent flexible substrate, uniformly spraying dispersion liquid containing conductive substances onto the transparent flexible substrate on which the mask plate is placed by using a spray gun to form a transparent conductive layer, controlling the shape of the mask plate to enable the transparent conductive layer to be composed of an area A and an area B, wherein the area A and the area B are separated by an interval channel and are not communicated with each other, and annealing to obtain a stable flexible patterned transparent conductive electrode;
(2) respectively spraying electrochromic polymers on the area A and the area B of the transparent conducting layer prepared in the step (1) by adopting a spraying method to form a first electrochromic layer and a second electrochromic layer, wherein the first electrochromic layer at least covers part of the area A, the second electrochromic layer at least covers part of the area B of the transparent conducting layer, and an interval channel between the area A and the area B is not sprayed with the electrochromic layer;
(3) and (3) coating a layer of gel electrolyte on the surface of the material obtained in the step (2) in a scraping mode, enabling the gel electrolyte layer to at least cover the first electrochromic layer, the second electrochromic layer and the area between the first electrochromic layer and the second electrochromic layer, drying the obtained device in an oven, and finally obtaining the electrochromic flexible display device with the parallel structure.
9. The method of claim 8, wherein: in the step (1), the annealing temperature is 40-60 ℃, and the annealing time is 30-60 min.
10. The method of claim 8, wherein: in the step (3), the drying temperature of the device is 40-70 ℃, and the drying time is 30-60 min.
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| CN108169975A (en) * | 2017-12-14 | 2018-06-15 | 江苏晟泰高新材料有限公司 | A kind of integrated electrochromic and the device and its laser processing of Electric double-layer capacitor structure |
| CN109521621A (en) * | 2018-12-28 | 2019-03-26 | 五邑大学 | A kind of electrochromic device of structure shoulder to shoulder and its application |
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| CN108169975A (en) * | 2017-12-14 | 2018-06-15 | 江苏晟泰高新材料有限公司 | A kind of integrated electrochromic and the device and its laser processing of Electric double-layer capacitor structure |
| CN109521621A (en) * | 2018-12-28 | 2019-03-26 | 五邑大学 | A kind of electrochromic device of structure shoulder to shoulder and its application |
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| CN113820898A (en) * | 2021-09-27 | 2021-12-21 | 苏州清越光电科技股份有限公司 | Electrochromic panel and preparation method thereof |
| CN113820898B (en) * | 2021-09-27 | 2024-02-02 | 苏州清越光电科技股份有限公司 | Electrochromic panel and preparation method thereof |
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