CN112255855A - Safe, environment-friendly and high-performance electrochromic film and preparation method thereof - Google Patents

Safe, environment-friendly and high-performance electrochromic film and preparation method thereof Download PDF

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CN112255855A
CN112255855A CN202011361470.2A CN202011361470A CN112255855A CN 112255855 A CN112255855 A CN 112255855A CN 202011361470 A CN202011361470 A CN 202011361470A CN 112255855 A CN112255855 A CN 112255855A
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safe
friendly
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electrochromic film
performance
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CN112255855B (en
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贾希来
巨小倩
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University of Science and Technology Beijing USTB
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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
    • G02F1/1523—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
    • 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
    • G02F1/1525—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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  • 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 discloses a preparation and test method of a safe, environment-friendly and high-performance electrochromic film capable of being applied to a water system electrolyte, and belongs to the field of electrochromic materials. The electrochromic film is a NiO film based on Ni-MOF, presents a spherical structure formed by stacking porous nano sheets, can be deposited on an ITO substrate through a simple hydrothermal method, and vertically grows on the ITO substrate, and has the diameter of about 2-10 mu m. The MOF derivative is used as the electrochromic material, and the porous structure of the MOF derivative enables the MOF derivative to be applied to an aqueous electrolyte system, so that the requirements on equipment are low, the raw materials are simple and easy to obtain, and the manufacturing cost is low. Provides possibility for preparing a water system electrochromic device with excellent performance, no toxicity, no pollution and low cost.

Description

Safe, environment-friendly and high-performance electrochromic film and preparation method thereof
Technical Field
The invention belongs to the field of electrochromic films, and particularly relates to a safe, environment-friendly and high-performance electrochromic material suitable for a water system electrolyte and a preparation method thereof.
Background
The electrochromic material realizes stable and reversible color change under the action of an external electric field, changes the optical properties of the material, such as reflectivity, absorptivity and the like, and thus realizes active adjustment of solar radiation transmittance. The electrochromic glass has excellent characteristics of light regulation and low energy consumption, so that the electrochromic glass can be widely applied to the aspects of intelligent building glass and has great advantages in the aspects of aerospace, automobile rearview mirrors, wearable equipment and the like.
The conventional electrochromic electrolyte is mainly an organic electrolyte, but the organic electrolyte has a great disadvantage in that it is generally strongly toxic and flammable, so that the organic electrolyte as an electrolyte for the electrochromic material may cause a serious safety problem. The aqueous electrolyte uses water to replace an organic solvent, so that the safety problem in the production process is improved, the environment is not polluted, and the electrochromic system is really green and safe. Thus, multivalent cations (e.g., Zn) compatible with aqueous electrolytes2+、Ca2+、Al3+Etc.) have come into the person's line of sight. The multivalent cation has more electrons than Li+Or any other monovalent ion, and therefore the aqueous electrolyte is expected to enhance the color contrast in addition to being safe and environmentally friendly.
However, most of the electrochromic materials reported are monovalent cations (such as H)+、Li+Etc.) ions with smaller diameter are taken as deintercalation ions, most of the deintercalation ions have compact structures and smaller pore diameters, and are not suitable for the deintercalation of multivalent cations with strong electrostatic action with a frame, thereby limiting the application of the water system electrolyte. Therefore, in order to expand the application of multivalent cations as an aqueous electrolyte for ion extraction, the development of nanomaterials having a mesoporous structure, a short ion diffusion distance, and a porous surface is of great value.
Disclosure of Invention
The invention aims to provide an electrochromic film which has larger pore diameter and a surface porous structure and can be suitable for an aqueous multivalent cation electrolyte and a preparation method thereof. According to the method, under the condition that the crystal is not prepared in advance, dense and uniform Ni-MOF grows on the ITO glass through a simple hydrothermal method, and the NiO electrochromic film is obtained after heat treatment and is suitable for a water system electrochromic system.
In order to achieve the purpose, the invention adopts the technical scheme that:
the electrochromic film is a NiO film based on Ni-MOF, presents a spherical structure formed by stacking porous nanosheets, vertically grows on an ITO substrate, and has the diameter of about 2-10 mu m.
Furthermore, the safe, environment-friendly and high-performance electrochromic film can realize reversible change between black and light colors in an aqueous electrolyte.
Further, the preparation method of the safe, environment-friendly and high-performance electrochromic film comprises the following specific steps:
step 1 first preparing a precursor solution: dissolving an organic ligand, metal salt and ultrapure water in an organic solvent, and stirring at normal temperature to obtain a precursor solution;
and 2, transferring the precursor solution obtained in the step 1 into a stainless steel autoclave, preparing a film on ITO glass by a hydrothermal method, washing, and annealing in a tubular furnace to obtain the safe, environment-friendly and high-performance electrochromic film.
And 3, taking the film obtained in the step 2 as a working electrode, a platinum wire as a counter electrode, an Ag/AgCl electrode as a reference electrode, and a salt water solution as an electrolyte to test the performance of the electrochromic film.
Further, in the step 1, the organic ligand is terephthalic acid, and the concentration of the organic ligand is 0.01-0.05 mol/L based on the precursor solution; the metal salt is nickel chloride hexahydrate, and the concentration of the metal salt is 0.01-0.05 mol/L based on the precursor solution.
Further, in the step 1, the organic solvent is N, N-dimethylformamide, and the volume ratio of the ultrapure water to the N, N-dimethylformamide is (1-1.5): 20.
further, the high-pressure reaction kettle in the step 2 is kept for 2-3 hours at the temperature of 110-130 ℃.
Further, in the step 2, the annealing temperature is 400-450 ℃, and the annealing time is 90-180 minutes.
Further, in the step 3, the aqueous electrolyte is one or a compound solution of two or three of an aqueous solution of aluminum chloride, an aqueous solution of zinc chloride and an aqueous solution of lithium chloride, and the test voltage range is 0-2V.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a method for preparing a safe, environment-friendly and high-performance electrochromic film with a simple preparation process, which has low requirements on equipment, simple and easily-obtained raw materials and low manufacturing cost.
2. According to the invention, MOFs is used as a template, and the derivatives of the MOFs can prevent metal ions from agglomerating and can be easily converted into a material with a porous nano structure with larger pores. The large aperture can weaken the electrostatic action between the crystal framework and ions, increase the contact area between the material and the electrolyte, increase the reaction active sites and shorten the ion transmission path, so that the film can be suitable for a water system electrolyte system.
3. The invention takes multivalent cations as de-intercalation ions, the multivalent cations support multi-electron redox reaction, and multiple electrons can be injected into the electrochromic material when the intercalation amount of the multivalent cations is the same as that of monovalent ions. This more efficient de-embedding approach can increase the response speed and achieve a larger light absorption modulation range within the same coloration time.
4. The invention can be applied to water system electrolyte, has high safety and no pollution, and is a green electrochromic system. And most of the used deintercalated ions are stored in the earth crust, are low in price, low in toxicity and easy to treat, and can be used as an effective substitute for lithium ion electrolyte.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a Scanning Electron Microscope (SEM) photograph of a safe, environmentally friendly and high performance electrochromic film prepared in example 1 of the present invention;
FIG. 2 is a diagram of a safe, environment-friendly and high-performance electrochromic film prepared in example 1 of the present inventionIn ZnCl2Transmittance before and after discoloration in the electrolyte was compared.
Detailed Description
For the convenience of understanding of those skilled in the art, the present invention will be further described with reference to the following drawings and examples, but the present invention is not limited thereto in any way.
Example 1
A preparation method of a safe, environment-friendly and high-performance electrochromic material comprises the following specific steps:
step 1, preparing a precursor solution at room temperature: 0.083g of terephthalic acid (0.5mmol) and 0.119g of nickel chloride hexahydrate (0.5mmol) were dissolved in 20ml of N, N-dimethylformamide at room temperature with stirring. 1mL of ultrapure water was slowly added to the solution during stirring.
And 2, transferring the precursor solution obtained in the step 1 into a stainless steel high-pressure autoclave, vertically soaking and fixing 2 x 2.5 ITO conductive glass in the precursor solution, keeping the solution at 120 ℃ for 3 hours, and cooling to room temperature after the reaction is finished. After washing, heating the sample to 450 ℃ in an argon atmosphere, keeping the temperature at 450 ℃ for 120 minutes, then replacing argon with air, continuing heating for 30 minutes, and changing the film from light green to light brown to obtain the NiO electrochromic film with the performance to be detected.
And 3, taking the film obtained in the step 2 as a working electrode, a platinum wire as a counter electrode, an Ag/AgCl electrode as a reference electrode, and a zinc chloride aqueous solution as an electrolyte to test the performance of the material electrochromic material in a voltage range of 0-1.1V. When the applied voltage is 0V, the film is in a fading state; when a voltage of 1.1V was applied, the film was colored.
Example 2
Step 1, preparing a precursor solution at room temperature: 0.083g of terephthalic acid (0.5mmol) and 0.119g of nickel chloride hexahydrate (0.5mmol) were dissolved in 20ml of N, N-dimethylformamide at room temperature with stirring. 1mL of ultrapure water was slowly added to the solution during stirring.
And 2, transferring the precursor solution obtained in the step 1 into a stainless steel high-pressure autoclave, vertically soaking and fixing 2 x 2.5 ITO conductive glass in the precursor solution, keeping the solution at 120 ℃ for 3 hours, and cooling to room temperature after the reaction is finished. After washing, heating the sample to 450 ℃ in an argon atmosphere, keeping the temperature at 450 ℃ for 120 minutes, then replacing argon with air, continuing heating for 30 minutes, and changing the film from light green to light brown to obtain the NiO electrochromic film with the performance to be detected.
And 3, taking the film obtained in the step 2 as a working electrode, a platinum wire as a counter electrode, an Ag/AgCl electrode as a reference electrode, and an aluminum chloride aqueous solution as an electrolyte to test the performance of the material electrochromic material in a voltage range of 0-1.1V. When the applied voltage is 0V, the film is in a fading state; when a voltage of 1.1V was applied, the film was colored.
The above are merely preferred examples of the present invention, and the scope of the present invention is not limited in any way. The technical solutions formed by local changes such as equivalent replacement and the like by those skilled in the art should be within the scope of the claims of the present invention.

Claims (10)

1. The safe, environment-friendly and high-performance electrochromic film is characterized in that the film is a NiO film based on Ni-MOF, presents a spherical structure formed by stacking porous nano sheets, is uniformly distributed on an ITO substrate, and has the diameter of 2-10 mu m, wherein continuous pore structures exist on the nano sheets.
2. The safe, environment-friendly and high-performance electrochromic film according to claim 1, wherein the electrochromic film has a nano-porous structure which enables the electrochromic film to be applied to an aqueous electrolyte and to realize reversible change between black and light colors.
3. The method for preparing the safe, environment-friendly and high-performance electrochromic film as claimed in claim 1, comprising the steps of:
step 1 first preparing a precursor solution: dissolving an organic ligand, metal salt and ultrapure water in an organic solvent, and stirring at normal temperature to obtain a precursor solution;
step 2, transferring the precursor solution obtained in the step 1 into a stainless steel autoclave, preparing a film on ITO glass by a hydrothermal method, and cooling to room temperature after the reaction is finished; after washing, annealing in a tubular furnace to obtain a safe, environment-friendly and high-performance electrochromic film;
and 3, taking the film obtained in the step 2 as a working electrode, a platinum wire as a counter electrode, an Ag/AgCl electrode as a reference electrode, and a salt water solution as an electrolyte to test the performance of the electrochromic film.
4. The preparation method of the safe, environment-friendly and high-performance electrochromic film according to claim 3, characterized in that: in the step 1, the organic ligand is terephthalic acid, and the concentration of the organic ligand is 0.01-0.05 mol/L.
5. The preparation method of the safe, environment-friendly and high-performance electrochromic film according to claim 3, characterized in that: in the step 1, the metal salt is nickel chloride hexahydrate, and the concentration of the metal salt is 0.01-0.05 mol/L.
6. The preparation method of the safe, environment-friendly and high-performance electrochromic film according to claim 3, characterized in that: in the step 1, the organic solvent is N, N-dimethylformamide, and the volume ratio of the ultrapure water to the N, N-dimethylformamide is (1-2): 20.
7. the preparation method of the safe, environment-friendly and high-performance electrochromic film according to claim 3, characterized in that: and (2) keeping the high-pressure reaction kettle at the temperature of 100-200 ℃ for 1-5 h.
8. The preparation method of the safe, environment-friendly and high-performance electrochromic film according to claim 3, characterized in that: in the step 2, the annealing temperature is 400-500 ℃, and the annealing time is 1.5-3 h.
9. The preparation method of the safe, environment-friendly and high-performance electrochromic film according to claim 3, characterized in that the aqueous electrolyte in the step 3 is one or a compound solution of two or three of an aqueous solution of aluminum chloride, an aqueous solution of zinc chloride and an aqueous solution of lithium chloride.
10. The method for preparing the safe, environment-friendly and high-performance electrochromic film according to claim 3, wherein the test voltage range in the step 3 is 0-2V.
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CN115079480A (en) * 2022-03-31 2022-09-20 中国人民解放军国防科技大学 Porphyrin MOF-based electrochromic film material and preparation method thereof
CN115340681A (en) * 2022-09-05 2022-11-15 浙江工业大学 Perylene bisimide derivative hybrid material, thin film and preparation method thereof
CN115612146A (en) * 2022-10-31 2023-01-17 辽宁大学 High-performance metal organic framework material and polyoxometallate electrochromic composite film and application thereof

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CN112745036A (en) * 2020-12-18 2021-05-04 北京工业大学 Preparation method of electrochromic film material with Ni-MOF-74 in-situ grown on ITO glass
CN115584031B (en) * 2022-10-14 2023-07-04 河南大学 Metal-organic framework material, film, preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN115079480A (en) * 2022-03-31 2022-09-20 中国人民解放军国防科技大学 Porphyrin MOF-based electrochromic film material and preparation method thereof
CN115079480B (en) * 2022-03-31 2023-12-29 中国人民解放军国防科技大学 Electrochromic film material based on porphyrin MOF and preparation method thereof
CN115340681A (en) * 2022-09-05 2022-11-15 浙江工业大学 Perylene bisimide derivative hybrid material, thin film and preparation method thereof
CN115340681B (en) * 2022-09-05 2023-11-03 浙江工业大学 Perylene bisimide derivative hybrid film and preparation method thereof
CN115612146A (en) * 2022-10-31 2023-01-17 辽宁大学 High-performance metal organic framework material and polyoxometallate electrochromic composite film and application thereof
CN115612146B (en) * 2022-10-31 2023-08-11 辽宁大学 High-performance metal organic framework material and polyoxometallate electrochromic composite film and application thereof

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