CN116540464A - Tungstate quantum dot-based hydrogel color-changing device with electrochromic function and photochromic function and preparation method thereof - Google Patents
Tungstate quantum dot-based hydrogel color-changing device with electrochromic function and photochromic function and preparation method thereof Download PDFInfo
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
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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
- G02F1/1514—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
- G02F1/15165—Polymers
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- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
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- G02B5/22—Absorbing filters
- G02B5/23—Photochromic filters
-
- 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
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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
- G02F1/157—Structural association of cells with optical devices, e.g. reflectors or illuminating devices
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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
- G02F1/163—Operation of electrochromic cells, e.g. electrodeposition cells; Circuit arrangements therefor
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- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention discloses a tungstate quantum dot-based hydrogel color-changing device with electrochromic and photochromic functions and a preparation method thereof, wherein the device comprises a working electrode/photochromic/electrolyte layer, an electrochromic layer and a counter electrode conductive layer; the working electrode/photochromic/electrolyte layer is acrylamide/2-acrylamide-2-methylpropanesulfonic acid/lithium chloride hydrogel with good ionic conductivity and good transparency and photochromic characteristics, the electrochromic layer is tungstate quantum dot/poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid composite solution which is prepared by spin coating, and the counter electrode conductive layer is acrylamide/2-acrylamide-2-methylpropanesulfonic acid hydrogel. The invention solves the technical problems that the existing color-changing device can not simultaneously realize electrochromic and photochromic, has rapid response speed, large transmittance adjustment, flexibility and the like.
Description
Technical Field
The invention belongs to the new material technology, and in particular relates to a tungstate quantum dot-based hydrogel with electrochromic and photochromic functions, a color-changing device and a preparation method thereof.
Background
Electrochromic and photochromic are phenomena that the optical characteristics of the material are reversibly and stably changed under the stimulation of an external electric field or an external light source, the electrochromic and photochromic materials can be mainly divided into organic color-changing materials and inorganic color-changing materials, the organic color-changing materials comprise spiropyrans, polythiophenes, viologens and derivatives thereof, the organic color-changing materials can realize the conversion among multiple colors, but the cycling stability is poor, the response sensitivity is low, and the requirements of daily increase in actual production and life cannot be met; inorganic color-changing materials have excellent thermal stability, chemical stability and reversible cycle property and are widely used, wherein tungsten oxide and tungstate are used as low-cost, nontoxic and environment-friendly inorganic materials, and have excellent electrochromic and photochromic characteristics, excellent optical contrast before and after color change and higher cycle stability, and are widely used in various fields. At present, research on preparing a color-changing material and a device by taking tungsten oxide and a tungstate material as electrochromic or photochromic elements is increasingly increased, and potential application prospects are shown in the fields of wearable electronic products, internet of things, intelligent windows and the like, but along with increasing demands on energy and management, the preparation and development of an electrochromic device with high-efficiency integration and multiple functions of electrochromic and photochromic are imperative, and although the color-changing device prepared by using common tungsten oxide or tungstate material has higher reversible circularity and chemical stability, the application of the device is limited due to long response time and poor optical contrast.
Disclosure of Invention
The invention discloses a tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions and a preparation method thereof, and solves the technical problems that the conventional color-changing device cannot simultaneously have both electrochromic and photochromic functions, high response speed, large transmittance adjustment, flexibility and the like.
The invention adopts the following technical scheme:
a tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions comprises a working electrode composite photochromic electrolyte layer, an electrochromic layer and a counter electrode conductive layer, wherein the electrochromic layer is positioned between the working electrode composite photochromic electrolyte layer and the counter electrode conductive layer.
In the invention, the working electrode composite photochromic electrolyte layer is acrylamide/2-acrylamide-2-methylpropanesulfonic acid/lithium chloride hydrogel; the electrochromic layer is a tungstate quantum dot/poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid composite layer; the counter electrode conductive layer is acrylamide/2-acrylamide-2-methylpropanesulfonic acid hydrogel.
The tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions comprises: a working electrode/photochromic/electrolyte layer, an electrochromic layer and a counter electrode conductive layer; the working electrode/photochromic/electrolyte layer is acrylamide/2-acrylamide-2-methylpropanesulfonic acid/lithium chloride hydrogel with good ionic conductivity and good transparency and photochromic characteristics, the electrochromic layer is tungstate quantum dot/poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid composite solution which is prepared by spin coating, and the counter electrode conductive layer is acrylamide/2-acrylamide-2-methylpropanesulfonic acid hydrogel. The tungstate quantum dot has excellent surface effect and small-size effect, enhances electrochromic and photochromic reactivity of the color-changing device, and has excellent flexibility, quick response capability and excellent electrochromic and photochromic characteristics.
The preparation method of the tungstate quantum dot-based hydrogel color-changing device with electrochromic and photochromic functions provided by the invention comprises the following steps:
(1) Preparing tungstate quantum dots by adopting a one-step hydrothermal method, and then mixing a tungstate quantum dot solution with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid, a surfactant and water to prepare a tungstate quantum dot/poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid electrochromic solution; preferably, the hydrothermal reaction temperature is 160-180 ℃ and the hydrothermal reaction time is 24-48h;
(2) Mixing tungstate quantum dots, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and lithium chloride to prepare acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride hydrogel which is a working electrode composite photochromic electrolyte layer, namely a working electrode/photochromic/electrolyte layer; preferably, acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, lithium chloride, tungstate quantum dots, ammonium persulfate, N-methylene bisacrylamide and water are mixed and stirred, and then transferred to a die for constant temperature drying to prepare a working electrode composite photochromic electrolyte layer; the mould and the transfer method are conventional techniques;
(3) Mixing acrylamide and 2-acrylamido-2-methylpropanesulfonic acid to prepare acrylamide/2-acrylamido-2-methylpropanesulfonic acid hydrogel, namely a counter electrode conducting layer; preferably, sequentially adding acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, ammonium persulfate and N, N-methylenebisacrylamide into an aqueous solution, stirring the mixture at room temperature, standing to remove bubbles, and drying at constant temperature to obtain a counter electrode conductive layer;
(4) Spin-coating electrochromic solution on the surface of a substrate to obtain an electrochromic layer, and respectively compounding a working electrode/photochromic/electrolyte layer and a counter electrode conductive layer on two sides of the electrochromic layer to prepare a hydrogel color-changing device; preferably, the spin coating speed is 1000-3000r/s; and (3) spin-coating the electrochromic solution on the surface of the ITO glass, and then performing high-temperature annealing treatment.
In the invention, in the electrochromic solution of tungstate quantum dots/poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid, the content of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid is 1.3-1.5%, the content of the solution of tungstate quantum dots is 14-15%, and the content of surfactant is 0.25-0.3% by mass.
The invention has the beneficial effects that:
(1) The tungstate quantum dots prepared by the hydrothermal method are simultaneously used as electrochromic units and photochromic units, and WO is adjusted 2- And H is + The tungstate quantum dots with different structures are prepared according to the molar ratio, the color-changing performance of the tungstate quantum dots can be regulated and controlled, and the preparation process is simple, the preparation cost is low, and the preparation method is safe and reliable.
(2) The all-solid-state flexible color-changing hydrogel device prepared by the invention is different from the traditional color-changing device, uses hydrogel as electrolyte and electrode material to replace the traditional liquid electrolyte and transparent conductive substrate (ITO, FTO and the like), solves the defects of difficult packaging, poor flexibility, complex assembly and the like of the traditional color-changing device, and widens the application prospect of the traditional color-changing device.
(3) The color-changing device prepared by the invention has excellent electrochromic and good photochromic behavior along with the change of sunlight intensity, namely, wide optical regulation range, short color-developing and fading response time, good cycling stability and the like.
Drawings
FIG. 1 is a schematic diagram of a method for preparing a tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions.
Fig. 2 is a transmission electron microscope picture of the tungstate quantum dots prepared in example 1.
FIG. 3 is a cross-sectional view of a scanning electron microscope of the ITO glass spin-on electrochromic layer prepared in example 1, wherein a is a low-magnification image and b is a high-magnification image.
FIG. 4 is a graph showing the transmittance of acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride hydrogels (AM/AMPS/LiCl), acrylamide/2-acrylamido-2-methylpropanesulfonic acid hydrogels (AM/AMPSl), acrylamide/lithium chloride hydrogels (AM/LiCl), and acrylic acid/acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride hydrogels (AA/APMS/AM/LiCl).
Fig. 5 is a graph showing transmittance before and after discoloration of the hydrogel discoloration devices prepared in example 1 and example 2.
Fig. 6 is a graph of transmittance of electrochromic layers (containing glass) prepared at different spin-on speeds.
Fig. 7 is a graph showing transmittance of electrochromic layers (including glass) prepared in example 1, example 2, and example 3.
FIG. 8 is a cyclic voltammogram of the electrochromic layer of the hydrogel color-changing device prepared in example 1 at different scan rates over an electrochemical window of-0.6V to 0.6V.
FIG. 9 is a graph showing the timing current of the hydrogel color-changing device prepared in example 1 at-0.6V to 0.6V.
FIG. 10 is a graph showing the timing current at-0.6V to 0.6V for the hydrogel color-changing device prepared in example 2.
FIG. 11 is a graph showing the timing current of the hydrogel color-changing device prepared in example 3 at-0.6V to 0.6V.
Detailed Description
At present, the research of preparing a color-changing material and a device by taking tungsten oxide and tungstate materials as electrochromic or photochromic elements is increasing, but the preparation of a high-efficiency integrated multifunctional color-changing device with electrochromic and photochromic functions still has great challenges. Meanwhile, the tungsten oxide and tungstate color-changing materials and devices prepared at present have the defects of long color switching response time, poor optical contrast, complex preparation process and the like. The invention aims to solve the technical problems that the existing color-changing device cannot simultaneously realize electrochromic and photochromic, has high response speed, large transmittance adjustment, flexibility and the like, and provides a tungstate quantum dot-based hydrogel color-changing device capable of simultaneously realizing electrochromic and photochromic and a preparation method thereof.
The tungsten oxide or tungstate is subjected to nano modification to prepare the tungstate quantum dot, so that the surface chemical activity of the tungstate quantum dot can be remarkably enhanced, the contact area between an electrochromic layer and electrolyte is increased, the insertion of ions is facilitated, the electrochromic time is shortened, and the responsiveness of the tungstate quantum dot is improved; meanwhile, the quantum effect of the tungstate quantum dots enables the tungstate quantum dots to generate photoelectron transfer faster under the stimulation of an external light source, the photochromic performance of the tungstate quantum dots is enhanced, an electrochromic solution is spin-coated on the surface of a substrate to obtain an electrochromic layer, and then a working electrode/photochromic/electrolyte layer is attached, so that the electrochromic layer is transferred; the electrochromic layer is attached to the opposite electrode conductive layer from the other side to prepare the hydrogel color-changing device, as shown in fig. 1, the tungstate quantum dots with excellent performance are prepared by a one-step hydrothermal method to serve as electrochromic and photochromic primitives, and the tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions is prepared by compounding the tungstate quantum dots with hydrogel, so that the tungstate quantum dot-based hydrogel color-changing device has wide application prospects in the fields of flexible sensing devices, wearable electronic equipment and the like.
The raw materials and the die adopted by the invention are existing products, and the specific preparation operation and the performance test are conventional technologies. Electrochromic: electrochromic performance of the devices was tested using the Shanghai Chenhua CHI650E electrochemical workstation chronoamperometry. The transmittance test method comprises the following steps: and measuring with ultraviolet-visible spectrophotometer at wavelength range of 250-800 nm. Coloring time and fade time determination: the time required for the device to stain and fade was measured with an ultraviolet-visible spectrophotometer at a wavelength of 550 nm. Optical contrast: the difference in transmittance of the device in the colored and discolored state at a wavelength of 550nm was measured with an ultraviolet spectrophotometer. Driving voltage: refers to the external voltage used to color and fade the device. Cyclic stability: the measurement was performed by electrochemical chronoamperometry.
Example 1
The preparation method of the tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions comprises the following steps:
(1) Dissolving 0.41g of sodium tungstate dihydrate in 25g of deionized water solution, adding 0.2534g of 0.1M hydrochloric acid solution after complete dissolution, adding 25mL of ethylene glycol, stirring and mixing to form a transparent colorless solution, transferring the transparent colorless solution into a 100mL polytetrafluoroethylene reaction kettle, heating and reacting for 48h in a 180 ℃ oven, and cooling to room temperature to prepare the tungstate quantum dot aqueous solution.
(2) 0.13g of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid solid, 1.4g of tungstate quantum dot solution and 0.025g of Triton-X100 solution are weighed and added into deionized water to prepare a 10g mixed solution, and the mixed solution is stirred and mixed for 1h to prepare the mixed electrochromic solution.
(3) Placing ITO glass in a surface plasma cleaning machine, and cleaning under the conditions that the cleaning condition is that the working power is 60W, the working pressure is 60Pa and the working time is 5 min; and (2) spin-coating the mixed electrochromic solution prepared in the step (2) on the surface of ITO glass, spin-coating for 30s at 3000r/s, and annealing at 120 ℃ for 10min. The above operation was repeated three times to prepare an electrochromic layer.
(4) The specific preparation method of the acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride photochromic hydrogel electrolyte and the electrode comprises the steps of dissolving 6g of acrylamide and 1.228g of 2-acrylamido-2-methylpropanesulfonic acid in 10g of deionized water, stirring and mixing for 10min, adding 2.95g of lithium chloride, 0.036g of ammonium persulfate and 0.025g of N, N-methylenebisacrylamide, continuously stirring for 20min, transferring to a mold, drying at a constant temperature in an oven at 60 ℃ for 1h, and cooling to room temperature to prepare the working electrode composite photochromic electrolyte layer.
(5) Attaching acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride photochromic hydrogel to the ITO glass surface with the electrochromic layer in the step (3), enabling the hydrogel surface to be in full contact with the electrochromic layer, standing for 10min at room temperature, and transferring the electrochromic layer from the ITO surface to the hydrogel surface through the adhesion performance between the electrochromic layer and the hydrogel surface.
(6) The preparation method of the acrylamide/2-acrylamido-2-methylpropanesulfonic acid hydrogel electrode comprises the following steps of dissolving 6g of acrylamide and 1.228g of 2-acrylamido-2-methylpropanesulfonic acid in 10g of deionized water, stirring and mixing for 10min, adding 0.036g of ammonium persulfate and 0.025g of N, N-methylenebisacrylamide, continuously stirring for 20min, transferring into a mold, drying at a constant temperature in a 60 ℃ oven for 1h, and cooling to room temperature to prepare the counter electrode conductive layer.
(7) The counter electrode conductive layer hydrogel and the working electrode composite photochromic hydrogel electrolyte layer transferred with the electrochromic layer form a close contact vertical layered structure in an attaching mode through the physical and chemical actions among the hydrogels, and the flexible all-solid-state hydrogel color-changing device is assembled.
As can be seen from the transmission electron microscope picture of fig. 2, the tungstate quantum dot solution prepared in example 1 shows a uniformly dispersed state in an aqueous solution.
As can be seen from fig. 3, the electrochromic solution was attached to the surface of the ITO glass by spin coating, and its thickness was about 2.5 um. The counter electrode conductive layer hydrogel and the photochromic/electrolyte layer working electrode hydrogel were both 3mm thick.
As can be seen from FIG. 4, the transmittance of the prepared acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride hydrogel was 91.54% (550 nm), and the transmittance of the acrylamide/2-acrylamido-2-methylpropanesulfonic acid hydrogel was 88.30% (550 nm).
As can be seen from fig. 5, the optical contrast of the prepared hydrogel color-changing device before and after color change was 70.61%.
As can be seen from fig. 6, the transmittance of the prepared electrochromic layer was 76%.
The electrochemical performance of the device adopts a double-electrode test method, the scanning speed of the cyclic voltammetry is 5, 10, 15 and 20mV/s, and the potential range is-0.6V-0.6V. As can be seen from fig. 8, the device exhibits a distinct redox peak and the larger the area encompassed by the cyclic voltammogram as the scan rate increases, indicating that as the scan rate increases, the more ion intercalation is facilitated, thereby storing more charge and thus increasing its areal capacitance.
The device circulation stability test adopts a double-electrode test method, the potential range of a timing current method is-1V-1V, the pulse time is 1s, and the static time is 2s. As can be seen from fig. 9, the prepared device was maintained stable in coloring current and fading current after being reversibly cycled about 1000 times, indicating that it has excellent reversible cycle.
As can be seen from table 1, the prepared device was excellent in electrochromic properties such as coloring and fading response time, optical contrast after coloring and fading, and driving voltage, and the like, and most of the electrochromic properties reported in the literature, indicating that it was excellent in electrochromic properties.
The spin coating speed of the mixed electrochromic solution in the step (3) was adjusted to 1000r/s or 2000r/s, and the transmittance of the obtained electrochromic layer was 67% and 72% respectively, as shown in fig. 6.
Example 2
The preparation method of the tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions comprises the following steps:
(1) In comparison with example 1, example 2 raised the amount of sodium tungstate dihydrate to 0.82g and the amount of 0.1m hydrochloric acid solution to 1.0g, and the other reagent amounts and preparation process were the same as in example 1.
(2) In example 2, the poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid solid was used in an amount of 0.065g compared to example 1. The other reagents were used in the same amounts and preparation as in example 1.
(3) The ITO glass cleaning step and annealing process were the same as in example 1. The spin coating process of the prepared mixed electrochromic solution spin-coated on the surface of the ITO glass comprises the following steps: spin-coating was repeated three times at 3000r/s for 30 s.
(4) The specific preparation method of the acrylamide/lithium chloride photochromic hydrogel electrolyte and the electrode comprises the following steps of dissolving 3.515g of acrylamide in 10g of deionized water, stirring and mixing for 10min, continuously stirring for 30min, transferring into a mold, drying at a constant temperature in a 60 ℃ oven for 1h, cooling to room temperature, soaking the hydrogel in 30% lithium chloride aqueous solution for 12h, wiping off surface water, and naturally drying for 4 h.
(5) The method of transferring the electrochromic layer on the surface of the ITO glass to the surface of the acrylamide/lithium chloride hydrogel was the same as in example 1. (6) The specific preparation method of the acrylamide/2-acrylamido-2-methylpropanesulfonic acid hydrogel electrode was the same as in example 1.
(7) The procedure for the flexible all-solid hydrogel color-changing device was the same as in example 1.
As can be seen from FIG. 4, the prepared acrylamide/lithium chloride hydrogel had a transmittance of 88.28% (550 nm) and exhibited excellent transparency.
As can be seen from FIG. 5, the optical contrast of the prepared hydrogel color-changing device before and after color change was 60.61%.
As can be seen from fig. 7, the transmittance of the prepared electrochromic layer was 66%.
The device circulation stability test adopts a double-electrode test method, the potential range of a timing current method is-1V-1V, the pulse time is 1s, and the static time is 2s. As can be seen from fig. 10, the prepared device has a certain attenuation of the coloring current and the fading current after being reversibly cycled for about 500 times, which indicates that the device has good reversible cyclicity.
Example 3
The preparation method of the tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions comprises the following steps:
(1) As compared to the preparation method of the tungstate quantum dot solution in example 1, 0.1545g of ammonium molybdate tetrahydrate solution was added, and other solvent amounts and preparation steps were the same as in example 1, with a small amount of ammonium molybdate added as a dopant.
(2) The preparation method of the mixed electrochromic solution is the same as in example 1.
(3) The ITO glass cleaning step and annealing process were the same as in example 1. The spin coating process of the prepared mixed electrochromic solution spin-coated on the surface of the ITO glass comprises the following steps: spin-coating was repeated three times at 3000r/s for 30 s.
(4) Preparation of acrylic acid/acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride photochromic hydrogel electrolyte and electrode in comparison with example 1, an acrylic acid solution was added in the method, and the total mass of acrylic acid and acrylamide was maintained at 6g, i.e., 2.84g of acrylic acid and 3.52g of acrylamide were added. The other reagents were used in the same amounts and preparation as in example 1.
(5) The procedure for transferring the electrochromic layer onto the surface of the acrylic acid/acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride hydrogel on the surface of the ITO glass was the same as in example 1.
(6) The specific preparation method of the acrylamide/2-acrylamido-2-methylpropanesulfonic acid hydrogel electrode was the same as in example 1.
(7) The procedure for the flexible all-solid hydrogel color-changing device was the same as in example 1.
As can be seen from FIG. 4, the transmittance of the prepared acrylic acid/acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride hydrogel was 91.38% (550 nm), showing excellent transparency.
As can be seen from fig. 7, the transmittance of the prepared electrochromic layer was 49%.
The device circulation stability test adopts a double-electrode test method, the potential range of a timing current method is-1V-1V, the pulse time is 1s, and the static time is 2s. As can be seen from FIG. 11, the prepared device showed a remarkable decay phenomenon of the coloring current and the fading current after being reversibly cycled for about 160 times, which indicates that the reversible cycle property is poor.
In Table 1, the references corresponding to the numbers 1-9 are as follows:
[1] CHEN C, LIU Y-H, ZHU M, et al. High-performance embedded nickel grid electrodes for fast-response and bendable all-solid PEDOT: PSS electrochromic devices [J]. Org Electron, 2020, 77.
[2] LV X, XU H, YANG Y, et al. Flexible laterally-configured electrochromic supercapacitor with feasible patterned display [J]. Chem Eng J, 2023, 458.
[3] ALMARRI A H. Enhanced electrochromic properties of anatase TiO2 for flexible electrochromic device [J]. Ionics, 2022, 28(9): 4435-4444.
[4] MA C, LIU H, TENG C, et al. Wetting-Induced Fabrication of Graphene Hybrid with Conducting Polymers for High-Performance Flexible Transparent Electrodes [J]. ACS Appl Mater Interfaces, 2020, 12(49): 55372-88381.
[5] KAI H, SUDA W, OGAWA Y, et al. Intrinsically Stretchable Electrochromic Display by a Composite Film of Poly(3,4-ethylenedioxythiophene) and Polyurethane [J]. ACS Appl Mater Interfaces, 2017, 9(23): 19513-19518.
[6] KIM D S, LEE Y H, KIM J W, et al. A stretchable array of high-performance electrochromic devices for displaying skin-attached multi-sensor signals [J]. Chem Eng J, 2022, 429.
[7] FAN Q, FAN H, LI K, et al. Stretchable, Electrochemically-Stable Electrochromic Devices Based on Semi-Embedded Ag@Au Nanowire Network [J]. Small, 2023: e2208234.
[8] YANG G, DING J, YANG B, et al. Highly stretchable electrochromic hydrogels for use in wearable electronic devices [J]. Journal of Materials Chemistry C, 2019, 7(31): 9481-9486.
[9] KIM Y, PARK C, IM S, et al. Design of intrinsically stretchable and highly conductive polymers for fully stretchable electrochromic devices [J]. Sci Rep, 2020, 10(1): 16488。
Claims (10)
1. a tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions comprises a working electrode composite photochromic electrolyte layer, an electrochromic layer and a counter electrode conductive layer, wherein the electrochromic layer is positioned between the working electrode composite photochromic electrolyte layer and the counter electrode conductive layer.
2. The electrochromic and photochromic tungstate quantum dot-based hydrogel color-changing device according to claim 1, wherein the working electrode composite photochromic electrolyte layer is an acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride hydrogel; the electrochromic layer is a tungstate quantum dot/poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid composite layer; the counter electrode conductive layer is acrylamide/2-acrylamide-2-methylpropanesulfonic acid hydrogel.
3. The method for preparing the electrochromic and photochromic tungstate quantum dot-based hydrogel color-changing device as set forth in claim 1, which is characterized by comprising the following steps:
(1) Preparing tungstate quantum dots by adopting a one-step hydrothermal method, and then mixing a tungstate quantum dot solution with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid, a surfactant and water to prepare a tungstate quantum dot/poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid electrochromic solution;
(2) Mixing tungstate quantum dots, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and lithium chloride to prepare acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride hydrogel serving as a working electrode composite photochromic electrolyte layer;
(3) Mixing acrylamide and 2-acrylamido-2-methylpropanesulfonic acid to prepare acrylamide/2-acrylamido-2-methylpropanesulfonic acid hydrogel which is a counter electrode conducting layer;
(4) Spin-coating an electrochromic solution on the surface of the substrate to obtain an electrochromic layer; and respectively compounding a working electrode/photochromic/electrolyte layer and a counter electrode conductive layer on two sides of the electrochromic layer to prepare the hydrogel color-changing device.
4. The method for preparing a tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions according to claim 3, wherein the hydrothermal reaction temperature is 160-180 ℃ and the hydrothermal reaction time is 24-48h; in the electrochromic solution of tungstate quantum dot/poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate, the content of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonate is 1.3-1.5%, the content of tungstate quantum dot solution is 14-15%, and the content of surfactant is 0.25-0.3%.
5. The method for preparing a tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions according to claim 3, wherein acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, lithium chloride, tungstate quantum dots, ammonium persulfate, N-methylene bisacrylamide and water are mixed and stirred, and then the mixture is dried at constant temperature to prepare the working electrode composite photochromic electrolyte layer.
6. The method for preparing a tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions according to claim 3, wherein acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, ammonium persulfate and N, N-methylenebisacrylamide are sequentially added into an aqueous solution, and the mixture is stirred at room temperature, then is left to stand for removing bubbles, and is dried at a constant temperature to prepare the counter electrode conductive layer.
7. The method for preparing a tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions according to claim 3, wherein the spin-coating speed is 1000-3000r/s; and (3) spin-coating the electrochromic solution on the surface of the ITO glass, and then performing high-temperature annealing treatment.
8. The preparation method of the working electrode composite photochromic electrolyte layer is characterized in that a one-step hydrothermal method is adopted to prepare tungstate quantum dots, and then tungstate quantum dot solution is mixed with poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid and surfactant to prepare a tungstate quantum dot/poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid electrochromic solution; then mixing tungstate quantum dots, acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and lithium chloride to prepare acrylamide/2-acrylamido-2-methylpropanesulfonic acid/lithium chloride hydrogel which is a working electrode composite photochromic electrolyte layer.
9. The use of the tungstate quantum dot-based hydrogel color-changing device with both electrochromic and photochromic functions as claimed in claim 1 for preparing a color-changing device or as a color-changing device.
10. Use of a working electrode composite photochromic electrolyte layer prepared by the method of claim 8 for preparing a tungstate quantum dot-based hydrogel photochromic device with both electrochromic and photochromic functions of claim 1.
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