CN116300232A - Multivalent ion electrolyte all-solid-state flexible electrochromic device and preparation method thereof - Google Patents

Multivalent ion electrolyte all-solid-state flexible electrochromic device and preparation method thereof Download PDF

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CN116300232A
CN116300232A CN202211101611.6A CN202211101611A CN116300232A CN 116300232 A CN116300232 A CN 116300232A CN 202211101611 A CN202211101611 A CN 202211101611A CN 116300232 A CN116300232 A CN 116300232A
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preparing
changing layer
color
film
solid
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陈曦
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Yangtze River Delta Research Institute of UESTC Huzhou
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Yangtze River Delta Research Institute of UESTC Huzhou
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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
    • G02F1/1506—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
    • G02F1/1523—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
    • G02F1/1524—Transition metal compounds
    • 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
    • G02F2001/1502—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 complementary cell

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Nonlinear Science (AREA)
  • Inorganic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)

Abstract

The invention relates to a multivalent ion electrolyte all-solid-state flexible electrochromic device and a preparation method thereof. The multivalent ion electrolyte film is prepared and pressed with the electrochromic layer and the complementary electrochromic layer in a hot pressing mode, so that the multivalent ion electrolyte all-solid-state flexible electrochromic device is prepared, the problem that a hard device is easy to damage is solved, and meanwhile, the safety of the electrochromic device in the preparation and use processes is improved.

Description

Multivalent ion electrolyte all-solid-state flexible electrochromic device and preparation method thereof
Technical Field
The invention relates to the technical field of chemical material synthesis and functional materials, in particular to a multivalent ion electrolyte all-solid-state flexible electrochromic device and a preparation method thereof.
Background
Electrochromic devices, because of their excellent optical properties, have been widely used in the fields of cell phone backplanes, camera obscuration, anti-glare automotive rearview mirrors, architectural smart windows, aircraft portholes, and the like. However, with popularization of application, the safety problems of the hard device after easy breakage and the safety problems of the electrolyte in the preparation and use processes have restricted the further development of the device.
Disclosure of Invention
Based on the problems in the background art, the invention provides a multivalent ion electrolyte all-solid-state flexible electrochromic device, which comprises a color-changing layer and a complementary color-changing layer which are oppositely arranged, and an electrolyte layer arranged between the color-changing layer and the complementary color-changing layer, wherein the color-changing layer, the electrolyte layer and the complementary color-changing layer are fixed through hot pressing.
The preparation method of the multivalent ion electrolyte all-solid-state flexible electrochromic device comprises the following steps of:
step one, processing a flexible conductive substrate: ultrasonically cleaning a flexible conductive substrate by adopting cleaning liquid, isopropanol and deionized water for 15min, drying, and then cleaning by using plasma for 10min;
step two, preparing an electrolyte layer: preparing solution with concentration of 0.1-2mol/L from magnesium salt, aluminum salt, calcium salt and Polycarbonate (PC) or water according to a certain proportion, then adding high polymer, stirring to form colloid, preparing film on a smooth flat plate in a coating mode, drying the prepared film in a vacuum oven, and stripping from the flat plate to obtain an electrolyte layer;
step three, preparing a color-changing layer: preparing a color-changing layer on the surface of the flexible conductive substrate treated in the first step by adopting a physical vapor deposition method; the preparation speed is 0.1-1 Emi/s, and the thickness of the prepared film is controlled to be 100-1000nm;
and step four, preparing a complementary color-changing layer: preparing a complementary color-changing layer on the surface of the flexible conductive substrate treated in the first step by adopting a physical vapor deposition method; the preparation speed is 0.1-1 Emi/s, and the thickness of the prepared film is controlled to be 100-1000nm.
Preferably, the flexible conductive substrate in the first step is PET or PMMA prepared with an ITO film, an AZO film, a CNT film, an Ag nanowire film.
Preferably, the magnesium salt in the second step is MgCl 2 、Mg(ClO 4 ) 2 Or Mg (PF) 6 ) 2 The method comprises the steps of carrying out a first treatment on the surface of the The aluminum salt is AlCl 3 、Al(ClO 4 ) 3 Or Al (PF) 6 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The saidThe calcium salt is CaCl 2 、Ca(ClO 4 ) 2 Or Ca (PF) 6 ) 2 The method comprises the steps of carrying out a first treatment on the surface of the The polymer is PMMA or PEG.
Preferably, the coating mode in the second step is blade coating, roll coating or spin coating; the smooth flat plate is glass or metal plate.
Preferably, the color-changing layer in the third step is a tungsten oxide film, a titanium dioxide film or a molybdenum oxide film.
Preferably, the complementary color-changing layer in the fourth step is a nickel oxide film or a vanadium oxide film.
Compared with the prior art, the invention has the beneficial effects that: the multivalent ion electrolyte film is prepared, and is pressed with the electrochromic layer and the complementary electrochromic layer by a hot pressing method, so that the multivalent ion electrolyte all-solid-state flexible electrochromic device is prepared, the problem that a hard device is easy to damage is solved, and meanwhile, the safety of the electrochromic device in the preparation and use processes is improved.
Drawings
Fig. 1 is a flow chart of the electrochromic device fabrication steps.
FIG. 2 is a spectral diagram of an electrochromic device.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The invention provides a multivalent ion electrolyte all-solid-state flexible electrochromic device and a preparation method thereof, which are implemented according to the following steps:
step one, processing a flexible conductive substrate: ultrasonically cleaning a flexible ITO-PET conductive substrate by adopting cleaning liquid, isopropanol and deionized water for 15min, drying, and then cleaning by using plasma for 10min;
step two, preparing an electrolyte layer: mg (ClO) 4 ) 2 Preparing a solution with the concentration of 0.1mol/L with Polycarbonate (PC), then adding high molecular PEG, stirring to form colloid, then preparing a film on a smooth glass plate in a blade coating mode, putting the prepared film into a vacuum oven for drying at 60 ℃, and stripping from the flat plate to obtain an electrolyte layer;
step three, preparing a color-changing layer: preparing a color-changing layer on the ITO surface of the step one by adopting a physical vapor deposition method; the preparation speed is 0.5 Emi/s, and the thickness of the prepared film is controlled at 450nm; the color-changing layer is a tungsten oxide film;
and step four, preparing a complementary color-changing layer: preparing a complementary color-changing layer on the ITO surface of the first step by adopting a physical vapor deposition method; the preparation speed is 0.5 Emi/s, and the thickness of the prepared film is controlled at 220nm; the complementary color-changing layer is a nickel oxide film;
step five, assembling devices: the device is assembled by adopting an assembly method of a sandwich structure, two films with a color-changing layer and a complementary color-changing layer are relatively stacked, an electrolyte layer is added in the middle, and hot pressing is carried out on the electrolyte layer, so that the multivalent ion electrolyte full-solid flexible electrochromic device can be obtained.
Example 2
The invention provides a multivalent ion electrolyte all-solid-state flexible electrochromic device and a preparation method thereof, which are implemented according to the following steps:
step one, processing a flexible conductive substrate: ultrasonically cleaning a flexible ITO-PET conductive substrate by adopting cleaning liquid, isopropanol and deionized water for 15min, drying, and then cleaning by using plasma for 10min;
step two, preparing an electrolyte layer: mg (ClO) 4 ) 2 Preparing a solution with the concentration of 0.1mol/L with Polycarbonate (PC), then adding high polymer PMMA, stirring to form colloid, preparing a film on a smooth glass plate in a roll coating mode, putting the prepared film into a vacuum oven for drying at 60 ℃, and stripping from the flat plate to obtain an electrolyte layer;
step three, preparing a color-changing layer: preparing a color-changing layer on the ITO surface of the step one by adopting a physical vapor deposition method; the preparation speed is 0.1 Emi/s, and the thickness of the prepared film is controlled at 450nm; the color-changing layer is a tungsten oxide film;
and step four, preparing a complementary color-changing layer: preparing a complementary color-changing layer on the ITO surface of the first step by adopting a physical vapor deposition method; the preparation speed is 0.1 Emi/s, and the thickness of the prepared film is controlled at 220nm; the complementary color-changing layer is a nickel oxide film;
step five, assembling devices: the device is assembled by adopting an assembly method of a sandwich structure, two films with a color-changing layer and a complementary color-changing layer are relatively stacked, an electrolyte layer is added in the middle, and hot pressing is carried out on the electrolyte layer, so that the multivalent ion electrolyte full-solid flexible electrochromic device can be obtained.
Example 3
The invention provides a multivalent ion electrolyte all-solid-state flexible electrochromic device and a preparation method thereof, which are implemented according to the following steps:
step one, processing a flexible conductive substrate: ultrasonically cleaning a flexible ITO-PET conductive substrate by adopting cleaning liquid, isopropanol and deionized water for 15min, drying, and then cleaning by using plasma for 10min;
step two, preparing an electrolyte layer: al (ClO) 4 ) 3 Preparing a solution with the concentration of 0.1mol/L with Polycarbonate (PC), then adding high polymer PMMA, stirring to form colloid, then preparing a film on a smooth glass plate in a blade coating mode, putting the prepared film into a vacuum oven for drying at 80 ℃, and stripping from the flat plate to obtain an electrolyte layer;
step three, preparing a color-changing layer: preparing a color-changing layer on the ITO surface of the step one by adopting a physical vapor deposition method; the preparation speed is 0.1 Emi/s, and the thickness of the prepared film is controlled at 1000nm; the color-changing layer is a tungsten oxide film;
and step four, preparing a complementary color-changing layer: preparing a complementary color-changing layer on the ITO surface of the first step by adopting a physical vapor deposition method; the preparation speed is 0.1 Emi/s, and the thickness of the prepared film is controlled at 300nm; the complementary color-changing layer is a nickel oxide film;
step five, assembling devices: the device is assembled by adopting an assembly method of a sandwich structure, two films with a color-changing layer and a complementary color-changing layer are relatively stacked, an electrolyte layer is added in the middle, and hot pressing is carried out on the electrolyte layer, so that the multivalent ion electrolyte full-solid flexible electrochromic device can be obtained.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.

Claims (7)

1. A multivalent ion electrolyte all-solid-state flexible electrochromic device characterized by: the color-changing device comprises a color-changing layer, a complementary color-changing layer and an electrolyte layer, wherein the color-changing layer and the complementary color-changing layer are oppositely arranged, the electrolyte layer is arranged between the color-changing layer and the complementary color-changing layer, and the color-changing layer, the electrolyte layer and the complementary color-changing layer are fixed through hot pressing.
2. A method of preparing a multivalent ion electrolyte all solid state flexible electrochromic device as claimed in claim 1, wherein the method of preparing is performed according to the steps of:
step one, processing a flexible conductive substrate: ultrasonically cleaning a flexible conductive substrate by adopting cleaning liquid, isopropanol and deionized water for 15min, drying, and then cleaning by using plasma for 10min;
step two, preparing an electrolyte layer: preparing solution with concentration of 0.1-2mol/L from magnesium salt, aluminum salt, calcium salt and Polycarbonate (PC) or water according to a certain proportion, then adding high polymer, stirring to form colloid, preparing film on a smooth flat plate in a coating mode, drying the prepared film in a vacuum oven, and stripping from the flat plate to obtain an electrolyte layer;
step three, preparing a color-changing layer: preparing a color-changing layer on the surface of the flexible conductive substrate treated in the first step by adopting a physical vapor deposition method; the preparation speed is 0.1-1 Emi/s, and the thickness of the prepared film is controlled to be 100-1000nm;
and step four, preparing a complementary color-changing layer: preparing a complementary color-changing layer on the surface of the flexible conductive substrate treated in the first step by adopting a physical vapor deposition method; the preparation speed is 0.1-1 Emi/s, and the thickness of the prepared film is controlled to be 100-1000nm.
3. The method for preparing the multivalent ion electrolyte all-solid-state flexible electrochromic device, according to claim 2, is characterized in that: the flexible conductive substrate in the first step is PET or PMMA prepared with an ITO film, an AZO film, a CNT film and an Ag nanowire film.
4. The method for preparing the multivalent ion electrolyte all-solid-state flexible electrochromic device, according to claim 2, is characterized in that: the magnesium salt in the second step is MgCl 2 、Mg(ClO 4 ) 2 Or Mg (PF) 6 ) 2 The method comprises the steps of carrying out a first treatment on the surface of the The aluminum salt is AlCl 3 、Al(ClO 4 ) 3 Or Al (PF) 6 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The calcium salt is CaCl 2 、Ca(ClO 4 ) 2 Or Ca (PF) 6 ) 2 The method comprises the steps of carrying out a first treatment on the surface of the The polymer is PMMA or PEG.
5. The method for preparing the multivalent ion electrolyte all-solid-state flexible electrochromic device, according to claim 2, is characterized in that: the coating mode in the second step is blade coating, roll coating or spin coating; the smooth flat plate is glass or metal plate.
6. The method for preparing the multivalent ion electrolyte all-solid-state flexible electrochromic device, according to claim 2, is characterized in that: and the color-changing layer in the third step is a tungsten oxide film, a titanium dioxide film or a molybdenum oxide film.
7. The method for preparing the multivalent ion electrolyte all-solid-state flexible electrochromic device, according to claim 2, is characterized in that: and the complementary color-changing layer in the fourth step is a nickel oxide film or a vanadium oxide film.
CN202211101611.6A 2022-09-09 2022-09-09 Multivalent ion electrolyte all-solid-state flexible electrochromic device and preparation method thereof Pending CN116300232A (en)

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CN202211101611.6A CN116300232A (en) 2022-09-09 2022-09-09 Multivalent ion electrolyte all-solid-state flexible electrochromic device and preparation method thereof

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CN116300232A true CN116300232A (en) 2023-06-23

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