CN113548809A - NiOxElectrochromic porous material and preparation method thereof - Google Patents
NiOxElectrochromic porous material and preparation method thereof Download PDFInfo
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
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- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/217—FeOx, CoOx, NiOx
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- C03C2217/20—Materials for coating a single layer on glass
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- C03C2217/241—Doped oxides with halides
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C03C2218/30—Aspects of methods for coating glass not covered above
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Abstract
The invention discloses a NiOxElectrochromic porous material and preparation method thereof, and NiOxThe electrochromic material has NiO with the average grain diameter of 40nmxPorous structure of particles prepared by preparing a NiOxNanoparticles and mixing NiOxPreparing an electrochromic sizing agent for a microelectronic printing blade coating system from nano particles, uniformly blade-coating the material on fluorine-doped tin oxide conductive glass by using a microelectronic printer to obtain electrochromic NiO with a certain thicknessxA film. The material has the characteristics of propylene carbonate/lithium perchlorate (PC/LiClO)4) The medium-color-change material has high fading state transmittance (78.3%) and low coloring state transmittance (24.1%), has a contrast ratio of over 54%, can realize reversible black and light yellow conversion under different voltages, can be used in the fields of intelligent windows and static display, and can realize the purpose of realizing nickel oxide in PC/LiClO4It becomes possible to form a complementary device with tungsten oxide in solution.
Description
Technical Field
The invention relates to the field of electrochromism, in particular to NiOxAn electrochromic porous material and a preparation method thereof.
Background
The electrochromic material is a material which can show reversible change among different colors through low voltage (generally < 5V) applied from the outside, and further realizes dynamic adjustment of absorption, transmission and reflectivity in visible light and infrared regions. The electrochromic material has the characteristics of low energy consumption, no pollution, no memory effect and no luminescence, so that the electrochromic material has good application prospects in the fields of intelligent windows, static display, infrared stealth and the like. Meanwhile, an ion embedding mechanism in the electrochromic reaction process enables the electrochromic material to have the same energy storage characteristic as a battery, so that the application of the electrochromic material in the direction of the dual-function device becomes possible. Electrochromic materials can be mainly classified into transition metal oxides, metal complexes, organic dye molecules, and organic conductive polymers. Among them, inorganic electrochromic materials have good electrochemical stability, environmental suitability and high contrast, and thus have become hot spots of research. Nickel oxide is a typical anodic inorganic electrochromic material and is one of the most widely used anodic coloring materials at present. Nickel oxide is inexpensive in raw material and exhibits high contrast in alkaline solutions, but it is one of the strong candidates for forming a complementary electrochromic device with tungsten oxide, in PC/LiClO4It is difficult to change color in the solution or the contrast is low. Therefore, how to prepare a polycarbonate/LiClO4The nickel oxide film which is remarkably discolored in the solution is one of the contents of the work of scientific research workers. In recent years, researchers have found that the oxygen content of nickel oxide is determined as to whether a nickel oxide thin film can be formed of PC/LiClO4Key to discoloration in solution, i.e., the higher the oxygen content, the higher the film is at PC/LiClO4The more pronounced the discoloration behavior in the solution. By heating in an argon-oxygen atmosphereThe magnetron sputtering technology can be used for preparing PC/LiClO4NiO with remarkable color changexThin films, but are expensive to commercialize due to their environmental severity (in vacuum) and complexity of the process.
Disclosure of Invention
The invention aims to provide NiOxAn electrochromic porous material and a preparation method thereof can prepare NiOxCoating the slurry on FTO to obtain PC/LiClO with loose porous structure4NiO with obvious color changing effect in solutionxAn electrochromic film.
In order to achieve the purpose, the invention provides the following technical scheme:
NiOxThe electrochromic porous material is formed by connecting nano particles in a network shape, has a porous structure, and has an average particle size of 30-50 nm.
Preferably, the NiO is formed by applying a low voltagexThe material can be in PC/LiClO4A fast transition between black and light yellow is achieved in the solution.
Preferably, the NiOxThe ratio of nickel to oxygen in the material is less than 1, and the initial state is pure black.
Preferably, the NiOxThe preparation method of the electrochromic porous material comprises the following steps:
(1) placing the FTO substrate in acetone, ethanol and deionized water in sequence for ultrasonic cleaning, placing the FTO substrate in an oven for drying after cleaning, and cleaning the FTO substrate in a UV light cleaning machine before use;
(2) preparation of NiOxPrecursor: preparing 3-5mol/L nickel nitrate ethanol solution in a beaker A, preparing NaOH aqueous solution with equal molar concentration in a beaker B, and slowly dripping the solution B into the solution A after the solution B is fully dissolved, wherein the dripping speed is 0.3-0.6 ml/s, so as to obtain green precipitate;
(3) repeatedly washing the green precipitate obtained in the step (2) with deionized water for 2-3 times, and drying in a drying oven at 80 ℃ for 12-18 h;
(4) preparation of NiOxPowder: fully grinding the product obtained in the step (3), and putting the product into a muffle furnace for calcining to obtain black NiOxPowder, the calcining temperature is 270-300 ℃, the heating rate is 1-5 ℃/min, and the heat preservation time is 60-180 min;
(5) dispersing the product obtained in the step (4) in a mixed solution of methanol and water, wherein the dispersion amount is 15-45mg/ml, and adding a proper amount of polyethylene glycol 4000;
(6) standing the product obtained in the step (5) for 2-4 days at the temperature of 10-25 ℃ to obtain a vertically layered solution;
(7) removing the supernatant of the product obtained in the step (6), adding a proper amount of polyethylene glycol 4000, and evaporating the solution to obtain viscous slurry;
(8) uniformly coating the product obtained in the step (7) on an FTO substrate in a microelectronic printer at a speed of 1-5mm/s, calcining for 0.5-1.5h on a heating platform at the calcining temperature of 270-xAn electrochromic film.
Preferably, it is characterized in that: the specific process of the step (1) is that the FTO is respectively cleaned in acetone, ethanol and deionized water for 15-30min, and then the FTO is dried in a drying oven at 60 ℃.
Preferably, the FTO of step (1) is cleaned in a 200W UV cleaner for 20-30min before use, so as to reduce the additional pressure value on the FTO surface, and make the slurry spread on the FTO surface more easily.
Preferably, the preparation of the mixed solution in the step (5) needs to add deionized water first and then add methanol, and the addition amount of the polyethylene glycol 4000 is not more than 0.1 g/ml.
Preferably, the residual volume of the supernatant of the product of step (7) does not exceed 10% of the sediment layer.
Preferably, the polyethylene glycol 4000 in the step (7) is added in an amount of 0.1g/ml to 0.3g/ml, when the amount is too low, the viscosity of the slurry is not enough, and when the amount is too high, the polyethylene glycol 4000 is easy to remain.
Preferably, the evaporation volume of the solution in the step (7) is between 1/4 and 1/2, and the kinematic viscosity is not lower than 50mm2/s。
Compared with the prior art, the invention has the beneficial effects that:
1. the invention prepares the powder into electronic slurry, evenly coats the slurry on an FTO substrate by scraping, and prepares NiO by adjusting the components of the slurryxElectrochromic film, NiOxThe electrochromic film consists of NiOxThe porous structure has larger specific surface area, greatly improves the diffusion rate of ions and the transmission speed of electrons, accelerates the reaction kinetics process, and improves the contrast and the response speed of the electrochromic film.
2、NiOxBlack, the proportion of oxygen content is greater than that of nickel, making it possible to use PC/LiClO4The solution has good color change effect and can form a complementary device with tungsten oxide; secondly, the material prepared by the invention has higher fading state transmittance (78.3%) and lower coloring state transmittance (24.1%), the contrast ratio of the material exceeds 54%, the reversible conversion of black and light yellow can be realized under different voltages, and the material can be used for intelligent windows and static display.
3. The polyethylene glycol 4000 is used for adjusting the viscosity of the slurry, so that the material has good adhesive force, can be effectively removed in the subsequent process, and promotes the film to form a porous structure.
4. The preparation method has the characteristics of simple process, controllable thickness, low cost and the like, and is favorable for industrial large-scale production.
Drawings
FIG. 1 shows NiO prepared in example 1 of the present inventionxAn X-ray diffraction pattern of the powder;
FIG. 2 shows NiO prepared in example 1 of the present inventionxA low-magnification electron microscope scanning image of the electrochromic porous film material;
FIG. 3 shows NiO prepared in example 1 of the present inventionxScanning a high-magnification electron microscope of the electrochromic porous film material;
FIG. 4 shows NiO prepared in example 1 of the present inventionxElectrochromic porous film material in PC/LiClO4Kinetic electrochromic behaviour diagram in solution (550nm ± 1 v);
FIG. 5 shows NiO prepared in example 2 of the present inventionxElectrochromic porous film material in PC/LiClO4The spectrum of the electrochromic property in the solution (250-1650 nm).
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
NiOxThe preparation method of the electrochromic porous film material comprises the following specific steps:
(1) and (3) placing the FTO substrate in acetone, ethanol and deionized water in sequence, ultrasonically cleaning for 30min, drying in a 60 ℃ oven after cleaning, and then placing in a 200W UV light cleaning machine for cleaning for 30 min.
(2) Preparation of NiOxPrecursor: preparing a 3mol/L nickel nitrate ethanol solution in a beaker A, preparing a 3mol/L NaOH aqueous solution in a beaker B, fully dissolving, slowly dropwise adding the solution B into the solution A at a dropwise adding speed of 0.5ml/s, stirring for 30min, and centrifuging at a speed of 6000rmp/min to obtain green NiOxAnd (4) precipitating a precursor.
(3) And (3) washing the green precipitate obtained in the step (2) with deionized water for 3 times, wherein the first washing needs to be centrifuged at 6000rmp/min, the second washing needs to be centrifuged at 8000rmp/min, the third washing needs to be centrifuged at 10000rmp/min, and after the washing is finished, drying the green precipitate in a drying oven at the temperature of 80 ℃ for 18 hours.
(4) Preparation of NiOxPowder: fully grinding the product obtained in the step (3), and putting the product into a muffle furnace for calcining to obtain black NiOxAnd (3) calcining the powder at 270 ℃, heating up at a rate of 2 ℃/min, and keeping the temperature for 120 min.
(5) And (3) taking 250mg of the product obtained in the step (4), dispersing in 5ml of water, adding 5ml of methanol and 0.6g of polyethylene glycol 4000, and stirring at the rotating speed of 800rpm for at least 8 hours.
(6) The product obtained in step (5) was allowed to stand in the environment (25 ℃) for 3 days to obtain a solution which was layered up and down.
(7) The supernatant of the product obtained in step (6) was removed by a dropper, 0.5g of polyethylene glycol 4000 was added thereto, and the 1/2 solution was evaporated at 80 ℃ to obtain a viscous slurry.
(8) Uniformly coating the product obtained in the step (7) on an FTO substrate in a microelectronic printer at the speed of 2mm/s, calcining for 0.5h on a heating platform at the temperature of 300 ℃, wherein the heating rate is 10 ℃/min, and naturally cooling to obtain black brown NiOxAn electrochromic film.
NiO prepared in this examplexElectrochromic porous film material with NiOxThe average particle size after film forming is about 40 nm. As can be seen from the XRD pattern, NiO was producedxThe phase structure of the nano powder is the same as that of pure NiO, no impurity phase is generated, and the particle size of the powder is about 16 nm. After film formation, the nanoparticles can agglomerate and form a porous structure. The dynamic spectrum of the electrochromic material prepared in the example is shown in fig. 4, and the contrast ratio of the electrochromic material reaches 54.1%, the coloring time is 1.1s, and the fading time is 1.7 s.
Example 2
NiOxThe preparation method of the electrochromic porous film material comprises the following specific steps:
(1) and (3) placing the FTO substrate in acetone, ethanol and deionized water in sequence, ultrasonically cleaning for 30min, drying in a 60 ℃ oven after cleaning, and then placing in a 200W UV light cleaning machine for cleaning for 30 min.
(2) Preparation of NiOxPrecursor: preparing 5mol/L nickel nitrate ethanol solution in a beaker A, preparing 5mol/L NaOH aqueous solution in a beaker B, after fully dissolving, slowly dripping the solution B into the solution A at the speed of 0.5ml/s, stirring for 30min, and centrifuging at the speed of 6000rmp/min to obtain green NiOxAnd (4) precipitating a precursor.
(3) And (3) washing the green precipitate obtained in the step (2) with deionized water for 2 times, wherein the first washing needs to be carried out at 6000rmp/min, the second washing needs to be carried out at 8000rmp/min, and the green precipitate is dried in a drying oven at 80 ℃ for 12 hours after being washed.
(4) Preparation of NiOxPowder: fully grinding the product obtained in the step (3), and putting the product into a muffle furnace for calcining to obtain black NiOxAnd (3) calcining the powder at 300 ℃, heating up at a rate of 5 ℃/min and keeping the temperature for 60 min.
(5) And (3) taking 300mg of the product obtained in the step (4), dispersing in 5ml of water, adding 5ml of methanol and 0.6g of polyethylene glycol 4000, and stirring at the rotating speed of 800rpm for at least 8 hours.
(6) The product obtained in step (5) was allowed to stand in the environment (25 ℃) for 3 days to obtain a solution which was layered up and down.
(7) The supernatant of the product obtained in step (6) was removed by a dropper, 0.8g of polyethylene glycol 4000 was added thereto, and the 1/3 solution was evaporated at 80 ℃ to obtain a viscous slurry.
(8) Uniformly coating the product obtained in the step (7) on an FTO substrate in a microelectronic printer at a speed of 4mm/s, calcining for 1h on a heating platform at the temperature of 300 ℃, wherein the heating rate is 10 ℃/min, and naturally cooling to obtain black brown NiOxAn electrochromic film.
NiO prepared in this examplexElectrochromic knife coating material with NiOxThe average particle size of the porous structure formed by the particles is about 40 nm. The spectrum of the electrochromic property of the electrochromic material prepared in this example is shown in fig. 5, and the contrast of the electrochromic material reaches 45.2%, the coloring time is 2.7s, and the fading time is 5.7 s.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the present invention as defined in the accompanying claims.
Claims (10)
1. NiOxAn electrochromic porous material is prepared from the electrochromic porous material,the method is characterized in that: the electrochromic film material is formed by connecting nano particles in a network shape, has a porous structure, and has an average particle size of 30-50 nm.
2. The NiO of claim 1xElectrochromic porous material, characterized in that: when a low voltage is applied, the NiOxThe material can be in PC/LiClO4A fast transition between black and light yellow is achieved in the solution.
3. The NiO of claim 2xElectrochromic porous material, characterized in that: the NiOxThe ratio of nickel to oxygen in the material is less than 1, and the initial state is pure black.
4. The NiO according to any one of claims 1 to 3xThe preparation method of the electrochromic porous material is characterized by comprising the following steps of:
(1) placing the FTO substrate in acetone, ethanol and deionized water in sequence for ultrasonic cleaning, placing the FTO substrate in an oven for drying after cleaning, and cleaning the FTO substrate in a UV light cleaning machine before use;
(2) preparation of NiOxPrecursor: preparing 3-5mol/L nickel nitrate ethanol solution in a beaker A, preparing NaOH aqueous solution with equal molar concentration in a beaker B, and slowly dripping the solution B into the solution A after the solution B is fully dissolved, wherein the dripping speed is 0.3-0.6 ml/s, so as to obtain green precipitate;
(3) repeatedly washing the green precipitate obtained in the step (2) with deionized water for 2-3 times, and drying in a drying oven at 80 ℃ for 12-18 h;
(4) preparation of NiOxPowder: fully grinding the product obtained in the step (3), and putting the product into a muffle furnace for calcining to obtain black NiOxPowder, the calcining temperature is 270-300 ℃, the heating rate is 1-5 ℃/min, and the heat preservation time is 60-180 min;
(5) dispersing the product obtained in the step (4) in a mixed solution of methanol and water, wherein the dispersion amount is 15-45mg/ml, and adding a proper amount of polyethylene glycol 4000;
(6) standing the product obtained in the step (5) for 2-4 days at the temperature of 10-25 ℃ to obtain a vertically layered solution;
(7) removing the supernatant of the product obtained in the step (6), adding a proper amount of polyethylene glycol 4000, and evaporating the solution to obtain viscous slurry;
(8) uniformly coating the product obtained in the step (7) on an FTO substrate in a microelectronic printer at a speed of 1-5mm/s, calcining for 0.5-1.5h on a heating platform at the calcining temperature of 270-xAn electrochromic film.
5. The NiO of claim 4xThe preparation method of the electrochromic porous material is characterized by comprising the following steps: the specific process of the step (1) is that the FTO is respectively cleaned in acetone, ethanol and deionized water for 15-30min, and then the FTO is dried in a drying oven at 60 ℃.
6. The NiO of claim 4xThe preparation method of the electrochromic porous material is characterized by comprising the following steps: cleaning the FTO in the step (1) in a 200W UV cleaning machine for 20-30min before use.
7. The NiO of claim 4xThe preparation method of the electrochromic porous material is characterized by comprising the following steps: and (3) preparing the mixed solution in the step (5) by adding deionized water and then adding methanol, wherein the addition amount of the polyethylene glycol 4000 is not more than 0.1 g/ml.
8. The NiO of claim 4xThe preparation method of the electrochromic porous material is characterized by comprising the following steps: the residual volume of the supernatant of the product obtained in the step (7) is not more than 10% of the precipitation layer.
9. The NiO of claim 4xThe preparation method of the electrochromic porous material is characterized by comprising the following steps: the polyethylene glycol 4000 is added in the step (7) in an amount of 0.1g/ml to 0.3g/mlBetween ml.
10. The NiO of claim 4xThe preparation method of the electrochromic porous material is characterized by comprising the following steps: the evaporation volume of the solution in the step (7) is 1/4-1/2, and the kinematic viscosity is not lower than 50mm2/s。
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| CN114163139A (en) * | 2021-12-23 | 2022-03-11 | 合肥工业大学 | Preparation method of composite nickel oxide film with two layers of different structures |
| CN114721198A (en) * | 2022-04-21 | 2022-07-08 | 合肥工业大学 | Quick-response flexible NiOx @ AgNWs electrochromic film and preparation method thereof |
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