CN112415826A - Method for simply and efficiently preparing multicolor all-solid-state electrochromic device - Google Patents
Method for simply and efficiently preparing multicolor all-solid-state electrochromic device Download PDFInfo
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- G02F1/1523—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material
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- G02F1/1525—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material characterised by a particular ion transporting layer, e.g. electrolyte
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Abstract
The invention discloses a method for simply and efficiently preparing a multicolor all-solid-state electrochromic device, which comprises the following steps: the tin dioxide/vanadium pentoxide electrochromic composite film is used as an electrochromic layer, and the polymer solid electrolyte is used as an ion conducting layer to rapidly assemble the all-solid-state electrochromic device through the ultraviolet curing effect. The polymer solid electrolyte takes polyethylene glycol diacrylate as a solvent, lithium bistrifluoromethanesulfonylimide as a solute, and the polyethylene glycol diacrylate is subjected to polycondensation reaction under the action of a photoinitiator to firmly combine the two electrodes. The polymer electrolyte exists in a liquid state before being solidified, so that the polymer electrolyte has good wettability when contacting with the electrochromic layer and the ion storage layer, and the purpose of fully contacting with the electrode material is achieved. The preparation method optimizes the device assembly process and provides a new direction and important reference for the design and preparation of the all-solid-state electrochromic device. Meanwhile, the device shows the same color change as the thin film single electrode, and is expected to be really applied to the military camouflage protection field.
Description
Technical Field
The invention relates to the technical field, in particular to a method for simply and efficiently preparing a multicolor all-solid-state electrochromic device.
Background
In the history of electrochromic technology research in almost sixty years, a great deal of research on materials and applications is carried out by scientific research works of various countries, and abundant experience is also accumulated. However, the method still has no wide application, is still in the stage of laboratory research, and has a long distance from the real commercial application and industrialization. From the viewpoint of device structure, each component has an influence on device performance, and optimization of each component is crucial. The design and assembly of electrochromic devices was the focus of research content at the beginning of the research in this field, and the application of materials also relies on the high-quality preparation of device products. The electrochromic device mainly comprises an electrochromic layer, an ion storage layer, an ion conducting layer, a transparent electrode and other materials, and the final performance of the device is determined by the excellent performance of the materials and has a great relationship with the assembly process of the device and the selection of each material. The performance requirements of the electrochromic device are as described above, such as high color contrast, fast response speed, good memory effect, stable cycle, etc. Tungsten trioxide and nickel oxide are typical cathodic and anodic electrochromic materials, respectively, and many of the previous studies have combined them together to form complementary devices. The performance improvement of the device mainly focuses on the optimization of the performance of the electrode material, such as the preparation of a material with a special appearance, the improvement of the film performance through element doping, the nano treatment of the material and the like. In addition, the selection of the electrolyte is also an important influencing factor, the liquid electrolyte has good wettability and is widely applied, but the sealing is difficult and the leakage is easy, in addition, the electrochromic device is mostly used in an open environment, and the electrolyte deterioration can also occur when the electrochromic device is exposed to sunlight. Solid electrolytes have a high safety factor because they do not have a problem of leakage as compared with liquid electrolytes, and have been widely studied and well-developed in the field related to battery energy in recent years. Considering the final application requirements of the research object, the preparation of all-solid-state electrochromic devices is the most possible method, and it is hoped that products with excellent performance and capable of being practically applied can be designed and prepared, so that a lot of experience and research ideas are provided for subsequent researches in the field.
Disclosure of Invention
To achieve the purpose, the invention provides a method for simply and efficiently preparing a multicolor all-solid-state electrochromic device. The preparation method has a simple and efficient assembly process, can be applied to various environments, and has good chemical stability and optical cycle performance. Meanwhile, the device can realize reversible conversion among yellow, green and blue, and has wide application prospect.
In the invention, a multicolor electrochromic film with a tin dioxide/vanadium pentoxide core-shell structure is selected as an electrochromic layer, FTO transparent conductive glass is selected as a counter electrode (ion storage layer), and a lithium bis (trifluoromethanesulfonylimide) polymer solid electrolyte is selected as an ion conductive layer to assemble the device simply and efficiently through ultraviolet curing. The polymer electrolyte generates strong binding force in the ultraviolet curing process, and the two electrodes of the device are quickly bonded into a whole, so that the assembly process is simplified, and uncertain factors influencing the performance of the device are reduced. The device is tested for electrochromic performance, has a fast coloring and fading speed and a high coloring rate, and can still maintain 71.7 percent of optical modulation after 100 cycles. The Lab chromaticity mode representation is carried out on different color states of the device, the color change similar to that of a thin film single electrode is displayed, and the device is expected to be applied to the military camouflage protection field. The design and preparation strategy of the all-solid-state electrochromic device provides a new direction and important reference for the development of multicolor solid-state devices in the future.
In order to achieve the purpose of the invention, the technical scheme provided by the invention is as follows:
a method for simply and efficiently preparing a multicolor all-solid-state electrochromic device comprises the following steps:
(1) ultrasonically cleaning a conductive substrate in water, and drying for later use;
(2) dissolving lithium bistrifluoromethanesulfonimide and 2-hydroxy-2-methyl propiophenone in polyethylene glycol diacrylate, and fully stirring until the lithium bistrifluoromethanesulfonimide and the 2-hydroxy-2-methyl propiophenone are dissolved to form a liquid polymer electrolyte;
(3) preparing a multicolor electrochromic film with a stannic oxide/vanadium pentoxide core-shell structure on a conductive substrate by combining a hydrothermal method and an electrodeposition method, carrying out plasma cleaning on the conductive substrate serving as an ion storage layer, and placing two electrodes in the air for later use;
(4) fixing the prepared conductive substrate coated with the multi-color electrochromic film with the tin dioxide/vanadium pentoxide core-shell structure by using a self-made clamp, and measuring a proper amount of the polymer electrolyte prepared in the step (2) to uniformly coat the polymer electrolyte on the electrochromic layer;
(5) and (4) placing the conductive substrate cleaned in the step (3) above the composite film electrode, tightly contacting with the electrolyte under the action of self gravity, starting an ultraviolet lamp for a certain time, taking the device out of the fixture after the ultraviolet lamp is completely cured, and cleaning a little electrolyte overflowing around the device to obtain the all-solid-state electrochromic device.
The following are preferred technical schemes of the invention:
in the step (1), the conductive substrate is ultrasonically cleaned in water and dried for standby, and the method specifically comprises the following steps:
ultrasonically cleaning the conductive substrate in a container filled with deionized water for 10-30 min, then drying the conductive substrate in a drying oven at 60 ℃, and performing surface treatment in a plasma cleaning machine for 3-10 min before performing hydrothermal reaction and device assembly.
The conductive substrate is FTO conductive glass, a conductive carbon cloth film or a conductive metal film. Further preferably, the FTO conductive glass is a commercially available product, the size of the FTO conductive glass can be customized, and the preparation of films with different areas is easy to realize.
In the step (2), the lithium bistrifluoromethanesulfonimide and the 2-hydroxy-2-methyl propiophenone are dissolved in the polyethylene glycol diacrylate and fully stirred until the lithium bistrifluoromethanesulfonimide and the 2-hydroxy-2-methyl propiophenone are dissolved to form a liquid polymer electrolyte, and the method specifically comprises the following steps: adding lithium bis (trifluoromethanesulfonyl) imide into polyethylene glycol diacrylate, stirring until the lithium bis (trifluoromethanesulfonyl) imide is completely dissolved, adding 2-hydroxy-2-methyl propiophenone, and stirring to dissolve to form a liquid polymer electrolyte.
The dosage ratio of the bis (trifluoromethane sulfonyl) imide lithium to the 2-hydroxy-2-methyl propiophenone to the polyethylene glycol diacrylate urea is 0.1 g-0.5 g: 5-20 μ L: 0mL to 3 mL.
And (3) in the process of carrying out plasma cleaning on the conductive substrate, ensuring that the conductive surface faces upwards, and the cleaning time is 5 min.
Further preferably, a power switch of the plasma cleaning machine is adjusted to a middle-gear working state.
In the step (4), the amount of the solid electrolyte required by the preparation of the device with a fixed size is 50-200 muL, and the device is uniformly coated and then kept stand to ensure full contact;
further preferably, the standing time is 5-10 min.
And (5) placing the ion storage layer on the polymer electrolyte, and controlling the stable state for a fixed time by using a clamp after the ion storage layer is completely contacted with the electrolyte under the self gravity.
Further preferably, the fixed time is 5-15 min, so that the electrolyte is ensured to be in full contact with the two electrodes.
Further preferably, in the step (5), the ultraviolet irradiation time required for curing the device is 3-10 min.
Preferably, the electrochromic device is all solid, the bis (trifluoromethane sulfonyl) imide lithium (LiTFSi) based polymer solid electrolyte is used as an ion conducting layer, the device is simply and efficiently assembled by utilizing the bonding force generated by ultraviolet curing, and the preparation process is optimized.
Preferably, the ultraviolet cured polymer solid electrolyte can be fully in wetting contact with the two electrode materials before solidification, which indicates that the fluidity of the electrolyte is better, and in addition, the conductive substrate subjected to plasma cleaning improves the wettability of the surface, improves the adhesive force of the film, and enhances the bonding force and stability of the device.
Preferably, the prepared all-solid-state electrochromic device has better performances in the aspects of coloring and fading speed, coloring efficiency, cycle performance and the like, can be reversibly transformed among yellow, green and blue, and can be applied to military self-adaptive camouflage in various environments.
Compared with the prior art, the invention has the following advantages:
1. the invention utilizes the binding force generated during the ultraviolet curing of the polymer to assemble the all-solid-state electrochromic device in one step, and provides a new idea for the design and preparation of the electrochromic device in the future. The prepared all-solid-state electrochromic device has strong binding force, and the integral stability of the device is improved. The electrolyte precursor has good fluidity, increases wetting fusion between the electrode and the electrolyte, and has positive influence on the performance of the device.
2. The polymer solid electrolyte has no influence on the reversible conversion performance of the composite film among yellow, green and blue, and the color diversity of the film material is continued on devices.
3. The excellent performance of the inorganic electrochromic material is applied to devices, and on the other hand, the inorganic electrochromic material provides supplement for the exploration of color change of electrochromic devices, and provides a new idea for realizing devices with three colors of yellow, green and blue.
4. The preparation method has the advantages of simplicity and high efficiency, and provides a new idea and reference experience on the assembly process of the electrochromic device.
5. The polymer electrolyte exists in a liquid state before being solidified, so that the polymer electrolyte has good wettability when contacting with the electrochromic layer and the ion storage layer, and the purpose of fully contacting with the electrode material is achieved. The preparation method optimizes the device assembly process and provides a new direction and important reference for the design and preparation of the all-solid-state electrochromic device. Meanwhile, the device shows the same color change as the thin film single electrode, and is expected to be really applied to the military camouflage protection field.
Drawings
FIG. 1 is a scanning electron photograph of the surface of an FTO conductive glass substrate and the surface of a solid electrolyte in contact with a tin dioxide/vanadium pentoxide composite film under different magnifications in example 2 of the invention;
FIG. 2 is a plot of chronoamperometry and corresponding in situ transmittance at a wavelength of 430nm for applied voltage intervals of-1V (30s) and 1V (30s) for an all-solid-state electrochromic device prepared in accordance with example 2 of the present invention;
fig. 3 is a graph of uv-vis spectral transmission of an all-solid electrochromic device prepared in example 2 according to the present invention in different operating states;
FIG. 4 is a graph of optical density as a function of embedded charge at 430nm for an all-solid-state electrochromic device prepared in example 2 of the present invention;
fig. 5 is a graph showing the results of the optical cycle stability test of the all-solid electrochromic device prepared in example 2 according to the present invention;
fig. 6 is a diagram showing the state change of a simple and efficient preparation of a multicolor all-solid-state electrochromic device in the present invention, which can reversibly change between blue (blue), yellow (colored) and green (intermediate).
Detailed Description
For the convenience of those skilled in the art, the present invention will be further described with reference to the accompanying drawings and examples.
Example 1
The method for simply and efficiently preparing the multicolor all-solid-state electrochromic device comprises the following steps:
ultrasonically cleaning FTO conductive glass (produced by Shenzhen south China Hunan science and technology company) in deionized water for 20 minutes, drying the cleaned FTO conductive glass in a 60 ℃ oven for standby, and treating the cleaned FTO conductive glass in a plasma cleaning machine for 5 minutes before hydrothermal reaction;
(2) dissolving 0.287g of lithium bis (trifluoromethanesulfonyl) imide in 1mL of polyethylene glycol diacrylate, fully stirring until the lithium bis (trifluoromethanesulfonyl) imide is dissolved, adding 10 mu L of 2-hydroxy-2-methyl propiophenone, and uniformly stirring to form a liquid polymer electrolyte for later use;
(3) firstly, preparing a multicolor electrochromic film with a stannic oxide/vanadium pentoxide core-shell structure on a conductive substrate as an electrochromic layer by combining a hydrothermal method and an electrodeposition method, then carrying out plasma cleaning on FTO conductive glass as an ion storage layer as the ion storage layer, and placing two electrodes in the air for later use;
(4) fixing the prepared FTO conductive glass coated with the multicolor electrochromic film with the tin dioxide/vanadium pentoxide core-shell structure by using a self-made clamp, measuring 50 microliter of the polymer electrolyte prepared in the step (2), uniformly coating the polymer electrolyte on an electrochromic layer, and standing for 10 min;
(5) and (4) placing the cleaned conductive substrate in the step (3) above the composite film electrode, tightly contacting with the electrolyte by utilizing the self gravity, starting an ultraviolet lamp for irradiating for 5min, taking the device out of the fixture after the device is completely cured, and cleaning a little electrolyte overflowing around the device to obtain the all-solid-state electrochromic device.
The all-solid-state electrochromic device prepared by the embodiment has strong binding force and overall stability, and as can be seen from fig. 1, the polymer solid electrolyte is fully contacted with the electrochromic layer and the ion storage layer, the electrolyte in a liquid state can be soaked into the electrode material with morphology, and a compact structure is formed under the ultraviolet curing action. Because the electrolyte is used in a relatively small amount, the formed solid electrolyte film is relatively thin, the distance for transmitting ions during work is short, and the device has certain advantages in coloring speed, but because the total amount of ions in the electrolyte is reduced, the device is not optimal in comprehensive performance, and the cycle performance is poor.
Example 2
The method for simply and efficiently preparing the multicolor all-solid-state electrochromic device comprises the following steps:
(1) ultrasonically cleaning FTO conductive glass (produced by Shenzhen south China Hunan science and technology company) in deionized water for 20 minutes, drying the cleaned FTO conductive glass in a 60 ℃ oven for standby, and treating the cleaned FTO conductive glass in a plasma cleaning machine for 5 minutes before hydrothermal reaction;
(2) dissolving 0.287g of lithium bis (trifluoromethanesulfonyl) imide in 1mL of polyethylene glycol diacrylate, fully stirring until the lithium bis (trifluoromethanesulfonyl) imide is dissolved, adding 10 mu L of 2-hydroxy-2-methyl propiophenone, and uniformly stirring to form a liquid polymer electrolyte for later use;
(3) firstly, preparing a multicolor electrochromic film with a stannic oxide/vanadium pentoxide core-shell structure on a conductive substrate as an electrochromic layer by combining a hydrothermal method and an electrodeposition method, then carrying out plasma cleaning on FTO conductive glass as an ion storage layer as the ion storage layer, and placing two electrodes in the air for later use;
(4) fixing the prepared FTO conductive glass coated with the multicolor electrochromic film with the tin dioxide/vanadium pentoxide core-shell structure by using a self-made clamp, measuring 100 mu L of the polymer electrolyte prepared in the step (2), uniformly coating the polymer electrolyte on an electrochromic layer, and standing for 10 min;
(5) and (4) placing the cleaned conductive substrate in the step (3) above the composite film electrode, tightly contacting with the electrolyte by utilizing the self gravity, starting an ultraviolet lamp for irradiating for 5min, taking the device out of the fixture after the device is completely cured, and cleaning a little electrolyte overflowing around the device to obtain the all-solid-state electrochromic device.
The all-solid-state electrochromic device prepared by the embodiment has strong binding force and overall stability, and as can be seen from fig. 1, the polymer solid electrolyte is fully contacted with the electrochromic layer and the ion storage layer, the electrolyte in a liquid state can be soaked into the electrode material with morphology, and a compact structure is formed under the ultraviolet curing action. From fig. 2, it can be known that the fading response time and the coloring response time of the all-solid-state electrochromic device are respectively 17s and 13s, and the response time meets the index requirement of military camouflage within 20 s. As shown in fig. 3, the transmittance curve of the device in three different operating states shows that the maximum transmittance modulation at 430nm is 43%, and the shape of the transmittance curve is determined by the different colors exhibited by the device in the different states. The data curve in fig. 4 shows the optical density of the device as a function of the amount of embedded charge at 430nm, and the coloring rate of the all-solid electrochromic device obtained by fitting the data of the curve is 31.4cm2 C-1The change of the color changing speed of the device is in corresponding relation with the coloring efficiency, and the performance is reduced compared with that of the composite film. The cycling curves shown in fig. 5 show that the all-solid state device can maintain an initial state optical modulation range of 71.7% after 100 cycles.
Example 3
The method for simply and efficiently preparing the multicolor all-solid-state electrochromic device comprises the following steps:
(1) ultrasonically cleaning FTO conductive glass (produced by Shenzhen south China Hunan science and technology company) in deionized water for 20 minutes, drying the cleaned FTO conductive glass in a 60 ℃ oven for standby, and treating the cleaned FTO conductive glass in a plasma cleaning machine for 5 minutes before hydrothermal reaction;
(2) dissolving 0.287g of lithium bis (trifluoromethanesulfonyl) imide in 1mL of polyethylene glycol diacrylate, fully stirring until the lithium bis (trifluoromethanesulfonyl) imide is dissolved, adding 10 mu L of 2-hydroxy-2-methyl propiophenone, and uniformly stirring to form a liquid polymer electrolyte for later use;
(3) firstly, preparing a multicolor electrochromic film with a stannic oxide/vanadium pentoxide core-shell structure on a conductive substrate as an electrochromic layer by combining a hydrothermal method and an electrodeposition method, then carrying out plasma cleaning on FTO conductive glass as an ion storage layer as the ion storage layer, and placing two electrodes in the air for later use;
(4) fixing the prepared FTO conductive glass coated with the multicolor electrochromic film with the tin dioxide/vanadium pentoxide core-shell structure by using a self-made clamp, measuring 200 microliter of the polymer electrolyte prepared in the step (2), uniformly coating the polymer electrolyte on an electrochromic layer, and standing for 10 min;
(5) and (4) placing the cleaned conductive substrate in the step (3) above the composite film electrode, tightly contacting with the electrolyte by utilizing the self gravity, starting an ultraviolet lamp for irradiating for 5min, taking the device out of the fixture after the device is completely cured, and cleaning a little electrolyte overflowing around the device to obtain the all-solid-state electrochromic device.
The all-solid-state electrochromic device prepared by the embodiment has strong binding force and overall stability, and as can be seen from fig. 1, the polymer solid electrolyte is fully contacted with the electrochromic layer and the ion storage layer, the electrolyte in a liquid state can be soaked into the electrode material with morphology, and a compact structure is formed under the ultraviolet curing action. The all-solid-state electrochromic device prepared in the embodiment shows different colors in different working states, as shown in table 1 and fig. 6, blue is shown in a fading state, green is shown in an intermediate state, yellow is shown in a coloring state, reversible transformation can be realized for three colors, and the color change of the film is verified by the Lab value of each color.
TABLE 1
The above-described embodiments of the present invention are modifications, improvements and decorations within the spirit and principle of the present invention, which should be considered as the protection scope of the present invention by those of ordinary skill in the art.
Claims (8)
1. A method for simply and efficiently preparing a multicolor all-solid-state electrochromic device is characterized by comprising the following steps of:
(1) ultrasonically cleaning a conductive substrate in water, and drying for later use;
(2) dissolving lithium bistrifluoromethanesulfonimide and 2-hydroxy-2-methyl propiophenone in polyethylene glycol diacrylate, and fully stirring until the lithium bistrifluoromethanesulfonimide and the 2-hydroxy-2-methyl propiophenone are dissolved to form a liquid polymer electrolyte;
(3) preparing a multicolor electrochromic film with a stannic oxide/vanadium pentoxide core-shell structure on a conductive substrate by combining a hydrothermal method and an electrodeposition method, carrying out plasma cleaning on the conductive substrate serving as an ion storage layer, and placing two electrodes in the air for later use;
(4) fixing the prepared conductive substrate coated with the multi-color electrochromic film with the tin dioxide/vanadium pentoxide core-shell structure by using a self-made clamp, and uniformly coating the liquid polymer electrolyte prepared in the step (2) on the electrochromic layer;
(5) the device is taken out from the clamp after the ultraviolet lamp is completely solidified, and the electrolyte overflowing around the device is cleaned up to obtain the multicolor all-solid-state electrochromic device.
2. The simple and efficient method for preparing a multicolor all-solid-state electrochromic device according to claim 1, wherein in the step (1), the conductive substrate is ultrasonically cleaned in water and dried for standby, and the method specifically comprises the following steps:
ultrasonically cleaning the conductive substrate in a container filled with deionized water for 10-30 min, then drying the conductive substrate in an oven at 50-70 ℃, and performing surface treatment in a plasma cleaning machine for 3-10 min.
3. The simple and efficient method for preparing a multicolor all-solid-state electrochromic device according to claim 1, wherein in the step (1), the conductive substrate is FTO conductive glass, a conductive carbon cloth film or a conductive metal film.
4. The simple and efficient method for preparing a multicolor all-solid-state electrochromic device according to claim 1, wherein in the step (2), the ratio of the amounts of lithium bistrifluoromethanesulfonylimide, 2-hydroxy-2-methyl propiophenone and polyethylene glycol diacrylate urea is 0.1 g-0.5 g: 5-20 μ L: 0mL to 3 mL.
5. The simple and efficient method for preparing multicolor all-solid-state electrochromic device according to claim 1, wherein in the step (4), the ratio of the amount of the liquid polymer electrolyte to the amount of the lithium bistrifluoromethanesulfonimide in the step (2) is 50 μ L-200 μ L: 0.1g to 0.5 g.
6. The simple and efficient method for preparing the multicolor all-solid-state electrochromic device according to claim 1, wherein in the step (4), the measured polymer electrolyte is uniformly coated on the electrochromic layer and then is kept still for 10-20 min.
7. The simple and efficient method for preparing a multicolor all-solid-state electrochromic device according to claim 1, wherein in the step (5), the ion storage layer is placed on the polymer electrolyte, and after the ion storage layer is completely contacted with the electrolyte under the self-gravity, the stable state is controlled by using a fixture for a fixed time.
8. The simple and efficient method for preparing a multicolor all-solid-state electrochromic device according to claim 1, wherein in the step (5), the irradiation time of the ultraviolet lamp is 3-10 min.
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| JP2005292819A (en) * | 2004-03-09 | 2005-10-20 | Fuji Photo Film Co Ltd | Nano-porous semiconductor material, optical density varying element, and camera unit |
| KR20120133739A (en) * | 2011-06-01 | 2012-12-11 | 한국이엔에쓰 주식회사 | UV curing gel-typed solid electrolyte for dye-sensitized solar cell |
| CN104698715A (en) * | 2013-12-04 | 2015-06-10 | 珠海兴业绿色建筑科技有限公司 | All-solid electrochromic device |
| CN109881198A (en) * | 2019-04-10 | 2019-06-14 | 浙江大学 | The preparation method of stannic oxide/vanadic anhydride core-shell structure multi-color electrochromic film |
| CN111073280A (en) * | 2019-11-25 | 2020-04-28 | 浙江工业大学 | Titanium dioxide/polyhexamethylene azanaphthalene triphenylamine core-shell structure composite film and preparation method and application thereof |
| CN111624828A (en) * | 2020-05-18 | 2020-09-04 | 电子科技大学 | Novel gel electrolyte and application thereof in all-solid-state electrochromic device |
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