CN115353701B - Preparation method and application of intelligent window foil capable of self-adapting to illumination intensity - Google Patents
Preparation method and application of intelligent window foil capable of self-adapting to illumination intensity Download PDFInfo
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- E06B9/00—Screening or protective devices for wall or similar openings, with or without operating or securing mechanisms; Closures of similar construction
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- E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
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- E06B9/00—Screening or protective devices for wall or similar openings, with or without operating or securing mechanisms; Closures of similar construction
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Abstract
The invention provides a preparation method and application of an intelligent window foil capable of adapting to illumination intensity, which comprises a carrier, photochromic inorganic nano particles and a catalyst, wherein the photochromic inorganic nano particles are converted from an oxidation state to a reduction state after absorbing sunlight so as to change the color self-adaptive sunlight intensity of the intelligent window foil from a light state to a dark state, and the photochromic inorganic nano particles are converted from the reduction state to the oxidation state when not absorbing sunlight so as to change the color self-adaptive sunlight intensity of the intelligent window foil from the dark state to a colorless state; the catalyst affects the sensitivity of the smart window foil to the adaptivity to light. The invention is suitable for large-area production, is transparent in colorless oxidation state and colored reduction state, can be attached to the existing window glass, does not need to replace the existing window, is convenient to use, has the advantages of flexibility, self-support, low cost, no scattering, energy conservation, environmental protection and the like, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of layered products, in particular to a preparation method and application of an intelligent window foil capable of self-adapting to illumination intensity.
Background
Along with the increasing importance of environmental protection and energy conservation, the sound of reasonable energy utilization is becoming larger, and meanwhile, the development and the development of energy-saving products are greatly progressed. Under such a background, earlier-80 years c.m. lampert and c.g. granqvist et al first proposed the application of electrochromic materials in energy-efficient lighting systems for buildings, automobiles, aircraft, etc., forming "smart windows" (smart windows) that can dynamically adjust solar radiation energy transmittance. In recent years, research and application of intelligent windows have been a hotspot of research.
At present, electrochromic intelligent windows based on tungsten trioxide or polymer dispersed liquid crystal are widely applied, but the electrochromic intelligent windows have complex device structures, high production cost and complex circuit devices, require extra energy consumption and cause certain potential safety hazards.
Therefore, passive thermochromic or photochromic smart windows that regulate their transmittance based on changes in temperature or light intensity of the environment are of great interest. The photochromic smart window is currently mainly based on organic photochromic dyes, which have the problems of poor stability and poor fatigue resistance. While photochromic inorganic nanoparticles exhibit good stability and fatigue resistance. The most representative of inorganic photochromic materials is tungsten trioxide. However, the preparation method of the inorganic photochromic intelligent window requires a high-temperature sintering process to limit the application of the inorganic photochromic intelligent window to a rigid substrate, or requires expensive high-vacuum magnetron sputtering equipment to be arranged on a flexible substrate, so that the manufacturing cost is increased, or the application of the intelligent window requires the replacement of the original common window, the operation is complex, the cost is high, and the like, so that the development of the intelligent window material is seriously hindered. In addition, the slow switching rate of the photochromic smart window between different transmittance is also a problem to be solved.
Therefore, it is important to develop an intelligent window foil based on inorganic photochromic nanoparticles, which can adapt to illumination intensity, so as to overcome the above problems.
Disclosure of Invention
The invention aims to solve the problems of cost and efficiency of photochromism, and provides a preparation method and application of an intelligent window foil capable of adapting to illumination intensity, when the intelligent window foil is used, an original window is not required to be replaced, the intelligent window foil is directly attached to the surface of a common window for use, the operation is simpler and more convenient, no external energy is consumed, and the intelligent window foil has the characteristics of flexibility, self-supporting, low cost, no scattering and the like; the preparation method has simple process, omits the modes of high-temperature sintering or high-vacuum magnetron sputtering and the like in the traditional preparation process, widens the application range and reduces the manufacturing cost; the intelligent window foil capable of self-adapting to illumination intensity is applied to the aspect of adjusting sunlight transmittance.
The invention provides an intelligent window foil capable of self-adapting to illumination intensity, which comprises a carrier and photochromic inorganic nano particles;
the carrier is used for uniformly distributing the photochromic inorganic nano particles;
the photochromic inorganic nano particles are used for converting the oxidation state into the reduction state after absorbing sunlight so as to enable the color self-adaptive sunlight intensity of the intelligent window foil to be changed from light to dark, and the photochromic inorganic nano particles are used for converting the reduction state into the oxidation state when not absorbing sunlight so as to enable the color self-adaptive sunlight intensity of the intelligent window foil to be changed from dark to light until reaching a colorless state.
The intelligent window foil capable of adapting to the illumination intensity, provided by the invention, is characterized in that the intelligent window foil further comprises a catalyst as an optimal way, and the catalyst is used for adjusting the conversion rate of the photochromic inorganic nano particles from a reduced state to an oxidized state.
According to the intelligent window foil capable of adapting to illumination intensity, as an optimal mode, the photochromic inorganic nano particles are made of wide-band gap semiconductor materials;
the photochromic inorganic nano-particles are any one of the following: titanium dioxide, tungsten trioxide and molybdenum trioxide;
the carrier is made of polymer which is colorless and transparent;
the intelligent window foil is of a transparent sheet structure.
According to the intelligent window foil capable of adapting to illumination intensity, as a preferable mode, the particle size of the photochromic inorganic nano particles is 2-10 nm, the weight ratio of the photochromic inorganic nano particles to the polymer is 5-10%, and the light absorption wave band of the photochromic inorganic nano particles is 250-400 nm;
the carrier is any one of the following: polymethyl methacrylate, polycarbonate and polystyrene;
the thickness of the intelligent window foil is 20-60 mu m.
The intelligent window foil capable of adapting to illumination intensity is characterized in that the catalyst is any one of the following materials: the weight ratio of the platinum, the copper chloride and the chromium chloride to the photochromic inorganic nano particles is 0-10%.
The invention provides a preparation method of an intelligent window foil capable of self-adapting to illumination intensity, which comprises the following steps:
s1, preparing sol: dissolving a precursor of the photochromic inorganic nano particles in a first solvent, and stirring to obtain sol;
s2, preparing solid sol: adding the sol into a second solvent containing a polymer, wherein the solubility of the photochromic inorganic nano-particles in the first solvent is larger than that in the polymer, and dispersing the photochromic inorganic nano-particles in the polymer by a solution supersaturation method to obtain solid sol;
s3, preparing an intelligent window foil: the solid solution glue solution is uniformly smeared on a glass substrate by using a coating method, and the intelligent window foil capable of adapting to the illumination intensity is obtained after drying and demoulding.
In the method for preparing the intelligent window foil capable of adapting to the illumination intensity, in the step S1, the first solvent is N, N-dimethylformamide, the concentration of the photochromic inorganic nano particles in the sol is 0.1-0.3 g/mL, and the stirring time is 1-3 h;
in step S2, the second solvent is dichloroethane, and the concentration of the polymer in the second solvent is: 0.2-0.6 g/mL;
in the step S3, the drying temperature is 40-70 ℃ and the drying time is 1-4 h.
The invention relates to a preparation method of an intelligent window foil capable of self-adapting to illumination intensity, which comprises the following steps as a preferable mode:
s1, preparing sol: dissolving a precursor of the photochromic inorganic nano particles and a catalyst in a first solvent, and stirring to obtain sol;
s2, preparing solid sol: adding the sol into a second solvent containing a polymer, wherein the solubility of the photochromic inorganic nano-particles in the first solvent is larger than that in the polymer, and dispersing the photochromic inorganic nano-particles in the polymer by a solution supersaturation method to obtain solid sol;
s3, preparing an intelligent window foil: the solid solution glue solution is uniformly smeared on a glass substrate by using a coating method, and the intelligent window foil capable of adapting to the illumination intensity is obtained after drying and demoulding.
According to the preparation method of the intelligent window foil capable of adapting to the illumination intensity, as a preferable mode, the first solvent is N, N-dimethylformamide, the concentration of the photochromic inorganic nano particles in the sol is 0.1-0.3 g/mL, the concentration of the catalyst in the sol is 0.02-0.03 g/mL, and the stirring time is 1-3 h;
in step S2, the second solvent is dichloroethane, and the concentration of the polymer in the second solvent is: 0.2-0.6 g/mL;
in the step S3, the drying temperature is 40-70 ℃ and the drying time is 1-4 h.
The invention relates to application of an intelligent window foil capable of self-adapting to illumination intensity, which is used for adjusting the transmittance of sunlight.
The invention relates to an intelligent window foil capable of self-adapting to illumination intensity, which comprises a polymer, photochromic inorganic nano particles and a catalyst;
polymers include, but are not limited to, colorless transparent polymethyl methacrylate, polycarbonate, polystyrene, and the like;
preferably, the polymer is polymethyl methacrylate;
photochromic inorganic nanoparticles include, but are not limited to, titanium dioxide, tungsten trioxide, molybdenum trioxide, and the like;
preferably, the photochromic inorganic nanoparticle is tungsten trioxide;
catalysts include, but are not limited to, platinum, copper chloride, chromium chloride, and the like;
preferably, the catalyst is cupric chloride;
preferably, the weight ratio of tungsten trioxide to polymethyl methacrylate is 5-10 wt%;
preferably, the weight ratio of the copper chloride to the tungsten trioxide is 0-10 wt%;
the absorption wave band of the tungsten trioxide is 250-400 nm;
the thickness of the intelligent window foil capable of adapting to the illumination intensity is 20-60 mu m.
The invention provides a preparation method of an intelligent window foil capable of self-adapting to illumination intensity, which comprises the following steps: dissolving a precursor of the photochromic inorganic nano particles in N, N-dimethylformamide, stirring to form sol, adding the sol into a solution containing a transparent polymer, stirring, and coating to obtain the intelligent window foil capable of adapting to illumination intensity;
the precursor of the photochromic inorganic nano-particles is chloride; preferably, the concentration of tungsten chloride in the sol is 0.1-0.3 g/mL; preferably, the concentration of polymethyl methacrylate in the polymethyl methacrylate-containing solution is 0.2-0.6 g/mL;
stirring time is 1-3 h, drying temperature is 40-70 ℃ and drying time is 1-2 h.
The invention provides an application of an intelligent window foil capable of self-adapting to illumination intensity in the aspect of regulating sunlight transmittance.
A first object of the present invention is to provide an intelligent window foil that is adaptable to the intensity of illumination. When the intelligent window foil is used, the intelligent window foil is directly attached to the surface of a common window without replacing an original window, is simpler and more convenient to operate, has no external energy consumption, and has the characteristics of flexibility, self-supporting, low cost, no scattering and the like.
A second object of the present invention is to provide a method for preparing a smart window foil as above which is adaptable to the illumination intensity. The preparation method has simple process, omits the modes of high-temperature sintering or high-vacuum magnetron sputtering and the like in the traditional preparation process, widens the application range and reduces the manufacturing cost.
A third object of the present invention is to provide an application of the intelligent window foil capable of adapting illumination intensity in adjusting solar light transmittance.
In order to achieve the first object, the present invention adopts the following technical scheme:
the invention discloses an intelligent window foil capable of self-adapting to illumination intensity, which comprises a polymer, inorganic photochromic nano particles and a catalyst.
According to the invention, the purpose of self-adaptive illumination intensity adjustment can be realized by adding the inorganic photochromic nano particles, the transparency can be changed along with the illumination intensity, when the illumination is strong, the transparency is reduced, the light transmission is reduced, the transparency is gradually recovered after the light intensity is reduced, and the polymer is used as the main component of the intelligent window foil to play a role in dispersing the photochromic material, so that the phenomenon of scattering of local light caused by aggregation due to uneven dispersion is avoided, and the intelligent window foil realizes a better effect of self-adaptive illumination intensity under the combined action of the inorganic photochromic nano particles and the transparent luminescent material.
The photochromic material provided by the invention comprises two different states of a colorless state and a coloring state, and can be in different states under different illumination intensities. Taking tungsten trioxide as an example, when the tungsten trioxide is in an oxidation state, the tungsten trioxide is absorbed in an ultraviolet light band and is not absorbed in a visible light band due to the characteristic of a wide-band gap semiconductor material, so that the intelligent window foil is in a transparent state. When the oxidized tungsten trioxide absorbs ultraviolet light, a pair of electrons and holes are generated, the electrons are re-injected into the tungsten trioxide and captured by oxygen vacancies, and the reduced W is generated 5+ The cavity is captured by water in the air to generate O 2 And H + ，H + Embedded in tungsten trioxide lattice to form HWO 3 Namely, the reduced tungsten trioxide, which is formed by capturing electrons by oxygen vacancies to form an F color center and scattering a large amount of free electrons, can have strong absorption to visible light and infrared light, so that the intelligent window foil is in a coloring state. When the tungsten trioxide in the reduced state is stopped being irradiated by ultraviolet light, oxygen in the air slowly oxidizes the tungsten trioxide in the reduced state to lead the tungsten trioxide to be removed from W 5+ Returning to W 6+ Corresponding H + Is extracted from tungsten trioxide crystal lattice to generate WO 3 And water, i.e. the reverse reaction of the photochromic reaction, the smart window foil reverts from the coloured state to the transparent state.
In the invention, the inorganic photochromic material is nano-scale, and the particle size of the inorganic photochromic material is 2-10 nm.
Further, the weight ratio of the inorganic photochromic material to the polymer is 5 to 10wt%.
Further, the weight ratio of the catalyst to the inorganic photochromic material is 0 to 10 percent by weight.
In order to better realize the effect of adapting to illumination intensity of the intelligent window foil, the inventor screens out a catalyst matched with the inorganic photochromic material through a large number of experiments, and the addition of the catalyst mainly influences the recovery rate of the photochromic material from a colored state to a colorless state, so that the sensitivity degree of the intelligent window foil to the adaptability to illumination is influenced, the sensitivity of the adaptability to illumination is improved, and the recovery time after color change is shortened. When no catalyst is added, the oxygen in the air is required to be oxidized slowly to realize the color fading of the intelligent window foil, and when the catalyst is introduced, the color fading process can be promoted, and the recovery process of the photochromic material can be accelerated. However, it will be understood by those skilled in the art that the discoloration process and the discoloration process of the smart window foil are in a competitive relationship, and the catalyst can be added to shorten the recovery rate after the discoloration, but the discoloration rate is reduced to some extent, and those skilled in the art can select whether to add the catalyst or not according to the needs.
When a catalyst exists in the system, taking copper chloride as an example, in the photochromic reaction process, part of generated photoelectrons are captured by oxygen vacancies of tungsten trioxide and part of photoelectrons are captured by Cu 2+ Absorption of Cu + ，Cu + Is in an unstable intermediate valence state and is more easily oxidized by oxygen in the air to generate Cu 2+ And Cu is 2+ Electrons trapped by the tungsten trioxide oxygen vacancies are absorbed, promoting the progress of the discoloration process.
Specifically, when tungsten trioxide absorbs ultraviolet light, W 6+ Is reduced to W 5+ ，Cu 2+ Is reduced to Cu + And after the light intensity becomes weak, cu + And W is 5+ Is oxidized back to Cu 2+ And W is 6+ The state allows the smart window foil to quickly recover the colorless oxidized state from the colored reduced state. In some preferred embodiments, the weight ratio of copper chloride to tungsten trioxide is 0wt%About 10wt%. Further preferably, the weight ratio of lithium iodide to tungsten trioxide includes, but is not limited to, 4wt%,5wt%,6wt%, and the like.
And, the doping amount of the photochromic nanomaterial can affect the initial transparency and the color-changing effect of the intelligent window foil. Taking tungsten trioxide and polymethyl methacrylate as examples, when the weight ratio of tungsten trioxide to polymethyl methacrylate exceeds 10wt%, significant aggregation occurs in the formed smart window foil, resulting in reduced transparency and uniformity of the entire film. When the weight ratio of tungsten trioxide to polymethyl methacrylate is less than 2wt%, the ultraviolet light irradiation has almost no photochromic effect. In some preferred embodiments, the weight ratio of tungsten trioxide to polymethyl methacrylate is from 5wt% to 10wt%. Further preferably, the weight ratio of tungsten trioxide to polymethyl methacrylate includes, but is not limited to, 7.5wt% and the like.
Further, the absorption band of the tungsten trioxide nano particles is 250-400 nm.
The thickness of the intelligent window foil is related to the solution concentration and the thickness of the liquid film in the coating process, and in order to ensure good practicality and manufacturing cost of the intelligent window foil, the thickness of the intelligent window foil is set to be 20-40 mu m.
In order to achieve the second object, the present invention adopts the following technical scheme:
the invention discloses a preparation method for preparing an intelligent window foil capable of self-adapting to illumination intensity, which comprises the following steps:
dissolving a precursor of the photochromic inorganic nano particles in N, N-dimethylformamide, stirring to form sol, adding the sol into a dichloroethane solution containing a polymer, uniformly stirring, uniformly coating the solution on a glass substrate by using a coating method, drying, and demolding to obtain the intelligent window foil capable of adapting to illumination intensity.
The formation of the photochromic inorganic nano particles directly affects the performance of the intelligent window foil capable of adapting to illumination intensity, the traditional nano particle preparation process such as a hydrothermal method and a ball milling method is not applicable to the preparation of the intelligent window foil, on one hand, the process has high energy consumption and complex operation, and has a certain danger, on the other hand, the prepared photochromic inorganic nano particles have large particle size, insignificant color change effect and poor compatibility with polymer matrixes, aggregation easily occurs in polymers, and more importantly, the invention not only aims at preparing the photochromic inorganic nano particles, but also needs a method capable of forming the photochromic inorganic nano particles under the intelligent window foil preparation system, so that the problem that the intelligent window foil meeting requirements cannot be prepared is solved, namely, the transparent and flexible intelligent window foil cannot be obtained by directly mixing the photochromic inorganic nano particles and the polymers, and the problem that the intelligent window foil cannot be automatically changed from colorless transparent to colored under the change of light intensity is solved. The method of supersaturation of the solution can be adopted to convert the precursor chloride into the photochromic inorganic nano particles in the intelligent window foil preparation system, and the photochromic inorganic nano particles are well dispersed in the polymer to form solid sol, so that the transition from the organic sol into the polymer solid sol is realized, the preparation process is reduced, the cost is reduced, the scattering phenomenon of light caused by the oversized or aggregated nano particles is avoided, and most importantly, the photochromic nano particles have good photochromic effect.
The supersaturation method of the solution is a method for preparing sol by utilizing the fact that the solubility of the same substance in different solvents is greatly different. The precursor chloride of the photochromic inorganic nano particles can be well dissolved in N, N-dimethylformamide, but has poor solubility in a polymer, and after the solvent is dried, the uniformly dispersed photochromic inorganic nano particles-polymer solid sol can be obtained.
In a specific embodiment, tungsten chloride is selected as a precursor of tungsten trioxide; copper chloride is selected as a catalyst; preferably, the concentration of tungsten chloride in the sol is 0.1-0.3 g/mL, and the concentration of copper chloride is 0.02-0.03 g/mL; preferably, the concentration of polymethyl methacrylate in the polymethyl methacrylate solution is 0.2-0.6 g/mL.
Further, the stirring time is 1 to 3 hours.
Further, the drying temperature is 50-70 ℃; the drying temperature is 1-4 h. In the selection of the drying temperature, the volatilization rate of the solvent is mainly considered, because the rapid volatilization of the solvent is a key for influencing the transparency of the intelligent window foil in the process of preparing the solid sol intelligent window foil by utilizing the solution supersaturation method, the solvent is excessively long in evaporation time, so that nanoparticles have larger probability of collision and aggregation in the film forming process, and finally the intelligent window foil scatters light; however, if the volatilization rate is too fast, volatile air holes are formed on the intelligent window foil when the solvent is removed, which also causes scattering of light by the intelligent window foil and affects the transmittance of the intelligent window foil, so that the drying temperature is controlled to be 50-70 ℃ to ensure that the drying process is completed within 1-4 hours, and in a specific embodiment, the set drying temperature is 60 ℃ and the drying time is 1 hour.
In order to achieve the third objective, the present invention discloses an application of the intelligent window foil capable of adapting to illumination intensity in adjusting sunlight transmittance.
When strong sunlight or sunlight simulator irradiates the intelligent window foil capable of adapting to illumination intensity, the transparency of the intelligent window foil is reduced, and light transmission is reduced. Specifically, when tungsten trioxide is simulated by sunlight (100 mW/cm 2 ) After 5min of irradiation, the transparent colorless smart window foil turned blue and darkened with increasing irradiation time. When the sunlight simulator is closed, the blue color of the intelligent window foil slowly disappears under the dark condition, and the intelligent window foil is restored to a colorless state.
The invention has the following advantages:
the invention discloses an intelligent window foil capable of self-adapting to illumination intensity, and preparation and application thereof. The smart window foil comprises a polymer, a photochromic inorganic nanoparticle and a catalyst, wherein the photochromic inorganic nanoparticle comprises a colorless oxidized state and a colored reduced state. After the photochromic inorganic nano particles absorb sunlight, the transition from a colorless oxidation state to a colored reduction state is realized, so that the intelligent window foil has light or dark color in self-adaptive sunlight intensity. After the catalyst is doped, the recovery rate of the photochromic inorganic nano particles can be influenced, and the sensitivity of the intelligent window foil to the adaptability of the illumination is further influenced. The intelligent window foil is transparent in the oxidation state and the colored reduction state, can be attached to the existing window glass, does not need to replace the existing window, is convenient to use, has the advantages of flexibility, self-support, low cost, no scattering, more energy conservation, environmental protection and the like, and has wide application prospects.
Drawings
FIG. 1 is a schematic diagram of a smart window foil with adaptive illumination intensity;
FIG. 2 is a flowchart of an embodiment 2 of a method for preparing an intelligent window foil with adaptive illumination intensity;
FIG. 3 is a flowchart of an embodiment 3 of a method for preparing an intelligent window foil with adaptive illumination intensity;
FIG. 4 is a schematic process diagram of the method of making the intelligent window foil of examples 4 and 5 with adaptive illumination intensity;
FIG. 5a is a schematic diagram showing macroscopic transparency of the smart window foil before irradiation with sunlight in example 4 of a method for preparing a smart window foil with adaptive illumination intensity;
FIG. 5b is a schematic diagram showing macroscopic transparency of the smart window foil after sunlight irradiation in example 4 of a method for preparing a smart window foil with adaptive illumination intensity;
FIG. 5c is a graph showing the transmittance of the intelligent window foil before and after irradiation with light in example 4, which is a method for preparing the intelligent window foil with adaptive illumination intensity;
FIG. 6a is a schematic diagram showing macroscopic transparency of the smart window foil before irradiation with sunlight in example 5 of a method for preparing a smart window foil with adaptive illumination intensity;
FIG. 6b is a schematic diagram showing macroscopic transparency of the smart window foil after sunlight irradiation in example 5 of a method for preparing a smart window foil with adaptive illumination intensity;
FIG. 6c is a graph showing the transmittance of the smart window foil before and after light irradiation in example 5, which is a method for preparing a smart window foil with adaptive illumination intensity;
FIG. 7a is a schematic illustration of a method for preparing an intelligent window foil with adaptive illumination intensity of 100mW cm for the intelligent window foils of examples 4 and 5 -2 365nm ultraviolet light of (2)A transmittance diagram of 0s of illumination under the lamp;
FIG. 7b is a schematic illustration of a method for preparing an intelligent window foil with adaptive illumination intensity of 100mW cm for the intelligent window foils of examples 4 and 5 -2 A transmittance diagram of 365nm ultraviolet light for 1 min;
FIG. 7c is a graph showing the preparation method of the intelligent window foil capable of adapting to the illumination intensity, wherein the intelligent window foil in examples 4 and 5 is 100mW cm -2 A transmittance diagram of 365nm ultraviolet light for 2 min;
FIG. 7d shows a method for preparing an intelligent window foil with adaptive illumination intensity, wherein the intelligent window foils in examples 4 and 5 are 100mW cm -2 A transmittance diagram of 365nm ultraviolet light for 3 min;
FIG. 7e shows a method for preparing an intelligent window foil with adaptive illumination intensity, wherein the intelligent window foils in examples 4 and 5 are 100mW cm -2 A transmittance diagram of 365nm ultraviolet light for 4 min;
FIG. 7f shows a method for preparing an intelligent window foil with adaptive illumination intensity, wherein the intelligent window foils in examples 4 and 5 are 100mW cm -2 A transmittance diagram of 365nm ultraviolet light for 5 min;
FIG. 7g is a graph showing the preparation method of the intelligent window foil capable of adapting to the illumination intensity, wherein the intelligent window foil in examples 4 and 5 is 100mW cm -2 A transmittance diagram of 365nm ultraviolet light for 10 min;
FIG. 7h shows a method for preparing an intelligent window foil with adaptive illumination intensity at 100mW cm in examples 4 and 5 -2 A transmittance diagram of 365nm ultraviolet light for 15 min;
FIG. 7i shows a method for preparing an intelligent window foil with adaptive illumination intensity, wherein the intelligent window foils in examples 4 and 5 are 100mW cm -2 A graph of the transmittance at 1050nm under an ultraviolet lamp of 365 nm;
FIG. 8a is a schematic diagram showing transmittance of the intelligent window foil in examples 4 and 5 for 0min during the recovery process of the discoloration of the intelligent window foil according to the preparation method of the intelligent window foil capable of adapting to the illumination intensity;
FIG. 8b is a schematic diagram showing transmittance of the intelligent window foil in examples 4 and 5 for 10min during the recovery process of the discoloration of the intelligent window foil according to the preparation method of the intelligent window foil capable of adapting to the illumination intensity;
FIG. 8c is a schematic diagram showing transmittance of the intelligent window foil in examples 4 and 5 for 20min during the recovery process of the color fading of the intelligent window foil according to the preparation method of the intelligent window foil capable of adapting to the illumination intensity;
FIG. 8d is a schematic diagram showing transmittance of the intelligent window foil in examples 4 and 5 for 30min during the recovery process of the fading of the intelligent window foil according to the preparation method of the intelligent window foil capable of adapting to the illumination intensity;
fig. 8e is a schematic diagram showing transmittance of the intelligent window foil in examples 4 and 5 for 40min in the process of recovering the color fading of the intelligent window foil according to the preparation method of the intelligent window foil capable of adapting to the illumination intensity;
FIG. 8f is a graph showing transmittance of the intelligent window foil in examples 4 and 5 for 50min during the recovery process of the discoloration of the intelligent window foil according to the preparation method of the intelligent window foil capable of adapting to the illumination intensity;
FIG. 8g is a graph showing transmittance of the intelligent window foil in examples 4 and 5 for 60min during the recovery process of the discoloration of the intelligent window foil according to the preparation method of the intelligent window foil capable of adapting to the illumination intensity;
FIG. 8h is a schematic diagram showing transmittance of the smart window foil in examples 4 and 5, which is recovered to the original state during the process of recovering the smart window foil from fading;
FIG. 8i is a graph showing the transmittance change at 1050nm of the smart window foil in examples 4 and 5 of the method for preparing a smart window foil with adaptive illumination intensity during the fade recovery of the smart window foil;
fig. 9 is a transmission electron microscope image of a smart window foil capable of adapting to illumination intensity, a preparation method thereof and a smart window foil in application example 4.
Fig. 10 is a transmission electron microscope image of a smart window foil with adaptive illumination intensity, a method for preparing the same, and a smart window foil of application example 5.
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.
Example 1
As shown in fig. 1, a smart window foil capable of adapting to illumination intensity comprises a carrier and photochromic inorganic nanoparticles;
the carrier is used for uniformly distributing the photochromic inorganic nano particles;
the photochromic inorganic nano particles are used for converting the oxidation state into the reduction state after absorbing sunlight so as to enable the color self-adaptive sunlight intensity of the intelligent window foil to be changed from shallow to deep, and the photochromic inorganic nano particles are used for converting the reduction state into the oxidation state when not absorbing sunlight so as to enable the color self-adaptive sunlight intensity of the intelligent window foil to be changed from deep to shallow until reaching a colorless state;
the components of the smart window foil further include a catalyst for adjusting a conversion rate of the photochromic inorganic nanoparticles from the reduced state to the oxidized state;
the particle diameter of the photochromic inorganic nano-particles is 2-10 nm, the weight ratio of the photochromic inorganic nano-particles to the polymer is 5-10%, and the light absorption wave band of the photochromic inorganic nano-particles is 250-400 nm;
the carrier is made of polymer, the polymer is colorless and transparent, and the polymer is any one of the following materials: polymethyl methacrylate, polycarbonate and polystyrene;
the photochromic inorganic nano-particles are wide-bandgap semiconductor materials;
the photochromic inorganic nano-particles are any one of the following: titanium dioxide, tungsten trioxide and molybdenum trioxide;
the intelligent window foil is of a transparent sheet structure, and the thickness of the intelligent window foil is 20-60 mu m;
the catalyst is any one of the following components: the weight ratio of the platinum, the copper chloride and the chromium chloride to the photochromic inorganic nano particles is 0-10%.
Example 2
As shown in fig. 2, a preparation method of an intelligent window foil capable of adapting to illumination intensity comprises the following steps: the method comprises the following steps:
s1, preparing sol: dissolving a precursor of the photochromic inorganic nano particles in a first solvent, and stirring to obtain sol; the precursor of the photochromic inorganic nano particles and the catalyst can be dissolved in a first solvent and stirred to obtain sol;
the precursor of the photochromic inorganic nano-particles comprises tungsten chloride, the first solvent is N, N-dimethylformamide, the concentration of the photochromic inorganic nano-particles in the sol is 0.1-0.3 g/mL, and the stirring time is 1-3 h;
the second solvent is dichloroethane, and the concentration of the polymer in the second solvent is: 0.2-0.6 g/mL;
s2, preparing solid sol: adding the sol into a second solvent containing a polymer, wherein the solubility of the photochromic inorganic nano-particles in the first solvent is larger than that in the polymer, and dispersing the photochromic inorganic nano-particles in the polymer by a solution supersaturation method to obtain solid sol;
s3, preparing an intelligent window foil: uniformly coating the solid solution glue solution on a glass substrate by using a coating method, and drying and demolding to obtain the intelligent window foil capable of adapting to the illumination intensity; the drying temperature is 40-70 ℃, and the drying time is 1-4 h.
Example 3
As shown in fig. 3, a preparation method of an intelligent window foil capable of adapting to illumination intensity comprises the following steps: the method comprises the following steps:
s1, preparing sol: dissolving a precursor of the photochromic inorganic nano particles and a catalyst in a first solvent, and stirring to obtain sol; the precursor of the photochromic inorganic nano particles and the catalyst can be dissolved in a first solvent and stirred to obtain sol, and the concentration of the catalyst in the sol is 0.02-0.03 g/mL;
the precursor of the photochromic inorganic nano-particles comprises tungsten chloride, the first solvent is N, N-dimethylformamide, the concentration of the photochromic inorganic nano-particles in the sol is 0.1-0.3 g/mL, and the stirring time is 1-3 h;
the second solvent is dichloroethane, and the concentration of the polymer in the second solvent is: 0.2-0.6 g/mL;
s2, preparing solid sol: adding the sol into a second solvent containing a polymer, wherein the solubility of the photochromic inorganic nano-particles in the first solvent is larger than that in the polymer, and dispersing the photochromic inorganic nano-particles in the polymer by a solution supersaturation method to obtain solid sol;
s3, preparing an intelligent window foil: uniformly coating the solid solution glue solution on a glass substrate by using a coating method, and drying and demolding to obtain the intelligent window foil capable of adapting to the illumination intensity; the drying temperature is 40-70 ℃, and the drying time is 1-4 h.
Example 4
As shown in fig. 4, a preparation method of an intelligent window foil capable of adapting to illumination intensity comprises the following steps: the method comprises the following steps:
0.3g of tungsten chloride (WCl) 6 ) And 0.015g of copper chloride (CuCl) 2 ) Dissolving in 1.5ml of N, N-Dimethylformamide (DMF), and stirring at room temperature for 2h to form sol for later use;
4g of polymethyl methacrylate (PMMA) are dissolved in dichloroethane, the PMMA concentration being 0.4 g.ml -1 Stirring for 2 hours at 60 ℃ for later use;
adding sol into dichloroethane solution of PMMA, stirring at room temperature for 2 hr, pouring onto glass substrate on the surface of coater, setting liquid film thickness to 200 μm, oven drying at 60deg.C for 1 hr, and demolding to obtain intelligent window foil (Cu-WO) capable of adapting to illumination 3 PMMA) the smart window foil has a thickness of 40 μm.
Example 5
As shown in fig. 4, a preparation method of an intelligent window foil capable of adapting to illumination intensity comprises the following steps: the method comprises the following steps:
0.3g of tungsten chloride (WCl) 6 ) Dissolving in 1.5ml of N, N-Dimethylformamide (DMF), and stirring at room temperature for 2h to form sol for later use;
4g were gatheredMethyl Methacrylate (PMMA) was dissolved in dichloroethane at a concentration of 0.4 g.ml -1 Stirring for 2 hours at 60 ℃ for later use;
adding sol into dichloroethane solution of PMMA, stirring at room temperature for 2 hr, pouring onto glass substrate with liquid film thickness of 200 μm, oven drying at 70deg.C for 1 hr, and demolding to obtain intelligent window foil (WO) capable of adapting to illumination 3 PMMA) the smart window foil has a thickness of 40 μm.
Example 6
0.14g of titanium tetrachloride (TiCl 4 ) And 0.015g of copper chloride (CuCl) 2 ) Dissolving in 1.5ml of N, N-Dimethylformamide (DMF), and stirring at room temperature for 2h to form sol for later use;
4g of polymethyl methacrylate (PMMA) are dissolved in dichloroethane, the PMMA concentration being 0.4 g.ml -1 Stirring for 2 hours at 60 ℃ for later use;
adding sol into dichloroethane solution of PMMA, stirring at room temperature for 2 hr, pouring onto glass substrate on the surface of coater, setting liquid film thickness to 200 μm, oven drying at 50deg.C for 1 hr, and demolding to obtain intelligent window foil (Cu-TiO) capable of adapting to illumination 2 PMMA) the smart window foil has a thickness of 40 μm.
Example 7
0.20g of molybdenum chloride (MoCl) 5 ) And 0.015g of copper chloride (CuCl) 2 ) Dissolving in 1.5ml of N, N-Dimethylformamide (DMF), and stirring at room temperature for 2h to form sol for later use;
4g of polymethyl methacrylate (PMMA) are dissolved in dichloroethane, the PMMA concentration being 0.4 g.ml -1 Stirring for 2 hours at 60 ℃ for later use;
adding sol into dichloroethane solution of PMMA, stirring at room temperature for 2 hr, pouring onto glass substrate on the surface of coater, setting liquid film thickness to 200 μm, oven drying at 60deg.C for 1 hr, and demolding to obtain intelligent window foil (Cu-MoO) capable of adapting to illumination 3 PMMA) the smart window foil has a thickness of 40 μm.
Example 8
0.3g of tungsten chloride (WCl) 6 ) And 0.015g of copper chloride (CuCl) 2 ) Dissolving in 1.5ml of N, N-Dimethylformamide (DMF), and stirring at room temperature for 2h to form sol for later use;
4g of Polycarbonate (PC) were dissolved in dichloroethane, the concentration of PC being 0.4 g.ml -1 Stirring for 2 hours at 60 ℃ for later use;
adding the sol into dichloroethane solution of PC, stirring at room temperature for 2 hr, pouring onto glass substrate on the surface of the coater, setting liquid film thickness to 200 μm, oven drying at 50deg.C for 1 hr, and demolding to obtain intelligent window foil (Cu-WO) capable of adapting to illumination 3 PC) the smart window foil has a thickness of 40 μm.
Example 9
0.3g of tungsten chloride (WCl) 6 ) And 0.015g of copper chloride (CuCl) 2 ) Dissolving in 1.5ml of N, N-Dimethylformamide (DMF), and stirring at room temperature for 2h to form sol for later use;
4g of Polystyrene (PS) was dissolved in dichloroethane, the PS concentration being 0.4 g.ml -1 Stirring for 2 hours at 70 ℃ for later use;
adding the sol into dichloroethane solution of PC, stirring at room temperature for 2 hr, pouring onto glass substrate on the surface of the coater, setting liquid film thickness to 200 μm, oven drying at 60deg.C for 1 hr, and demolding to obtain intelligent window foil (Cu-WO) capable of adapting to illumination 3 PS), the smart window foil has a thickness of 40 μm.
The smart window foils of examples 4 to 5 were exposed to sunlight for 10 minutes, and the transparency changes are shown in fig. 5a, 5b, 6a, and 6 b. The intelligent window foil is completely transparent before illumination, and is marked as colorless, the color of the film is deepened after illumination, and the transmittance of light is obviously reduced, and is marked as colored. As shown in fig. 5c and 6c, the transparent spectrum and the reflection spectrum of the smart window foil represent that the smart window foil in a colorless state only absorbs ultraviolet light, and the smart window foil in a colored state strongly absorbs ultraviolet light, visible light and infrared light. The intelligent window foil is placed under a sunlight simulator with the power of 100mW cm -2 For 15min, its coloring process and its color fading recovery process transparencyThe changes are shown in figures 7 a-7 h and 8 a-8 h, the transparency of the two films is slowly reduced along with the illumination time, the transparency is gradually recovered along with the time after no illumination, and the Cu-WO doped with the catalyst copper chloride can be seen 3 The discoloration time of the PMMA smart window foil was about 1h, whereas WO without the catalyst copper chloride was used 3 The PMMA smart window foil has little discoloration in 1h. The transmittance at 1050nm in the color change and color fading process is changed along with the illumination time as shown in FIG. 7i and FIG. 8i, and the intelligent window foil is placed under 365nm ultraviolet light at 5mW cm -2 The transmittance of the Cu-WO doped with the catalyst copper chloride after the light source is turned off is gradually reduced along with the irradiation time after 180s of power irradiation 3 The transmittance of the/PMMA smart window foil slowly returns to the original state within 1h, while the WO without the catalyst copper chloride doped 3 The transmittance of the/PMMA smart window foil was only restored to 40% within 1h.
The intelligent window foils of examples 4 to 5 were sectioned and observed under a transmission electron microscope, and as shown in fig. 9 and 10, the distribution of tungsten trioxide nanoparticles in the intelligent window foil and the particle size of the particles were about 20nm were seen.
The same effects can be achieved in examples 1 to 2 and 6 to 9.
Example 10
The application of the intelligent window foil capable of self-adapting to illumination intensity is applied to adjusting the transmittance of sunlight.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (8)
1. A preparation method of an intelligent window foil capable of self-adapting to illumination intensity is characterized by comprising the following steps:
the intelligent window foil capable of self-adapting to illumination intensity comprises a carrier and photochromic inorganic nano particles;
the carrier is used for uniformly distributing the photochromic inorganic nano particles;
the photochromic inorganic nano particles are in an oxidation state and a reduction state, the oxidation state is in a colorless state, the reduction state is in a coloring state, the photochromic inorganic nano particles are used for converting the oxidation state into the reduction state after absorbing sunlight so as to enable the color self-adaptive sunlight intensity of the intelligent window foil to be changed from light to deep, and the photochromic inorganic nano particles are used for converting the reduction state into the oxidation state when the sunlight cannot be absorbed so as to enable the color self-adaptive sunlight intensity of the intelligent window foil to be changed from deep to light until reaching the colorless state;
the preparation method of the intelligent window foil capable of adapting to the illumination intensity comprises the following steps:
s1, preparing sol: dissolving a precursor of the photochromic inorganic nano particles in a first solvent, and stirring to obtain sol;
s2, preparing solid sol: adding the sol into a second solvent containing a polymer, wherein the solubility of the precursor of the photochromic inorganic nano particles in the first solvent is larger than that in the polymer, and dispersing the photochromic inorganic nano particles in the polymer by a solution supersaturation method to obtain a solid sol;
s3, preparing an intelligent window foil: uniformly coating the solid solution glue solution on a glass substrate by using a coating method, drying and demolding to obtain the intelligent window foil capable of adapting to illumination intensity, wherein the drying temperature is 40-70 ℃, and the drying time is 1-4 hours;
the particle size of the photochromic inorganic nano particles is 2-10 nm, the weight ratio of the photochromic inorganic nano particles to the polymer is 5-10%, and the light absorption wave band of the photochromic inorganic nano particles is 250-400 nm;
the carrier is any one of the following: polymethyl methacrylate, polycarbonate and polystyrene;
the thickness of the intelligent window foil is 20-60 mu m.
2. The method for preparing the intelligent window foil capable of adapting to illumination intensity according to claim 1, wherein the method comprises the following steps: the composition of the smart window foil further includes a catalyst for adjusting a rate of conversion of the photochromic inorganic nanoparticles from the reduced state to the oxidized state.
3. The method for preparing the intelligent window foil capable of adapting to illumination intensity according to claim 1, wherein the method comprises the following steps: the photochromic inorganic nano particles are any one of the following: titanium dioxide, tungsten trioxide and molybdenum trioxide;
the intelligent window foil is of a transparent sheet structure.
4. The method for preparing the intelligent window foil capable of adapting to illumination intensity according to claim 2, which is characterized by comprising the following steps: the catalyst is any one of the following: the weight ratio of the catalyst to the photochromic inorganic nano particles is 0-10%.
5. The method for preparing the intelligent window foil capable of adapting to illumination intensity according to claim 1, wherein the method comprises the following steps: in the step S1, the first solvent is N, N-dimethylformamide, the concentration of the photochromic inorganic nanoparticle precursor in the sol is 0.1-0.3 g/mL, and the stirring time is 1-3 h;
in step S2, the second solvent is dichloroethane, and the concentration of the polymer in the second solvent is: 0.2 to 0.6g/mL.
6. The method for preparing the intelligent window foil capable of adapting to illumination intensity according to any one of claims 2 and 4, which is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing sol: dissolving a precursor of the photochromic inorganic nano particles and a catalyst in a first solvent, and stirring to obtain sol;
s2, preparing solid sol: adding the sol into a second solvent containing a polymer, wherein the solubility of the precursor of the photochromic inorganic nano particles in the first solvent is larger than that in the polymer, and dispersing the photochromic inorganic nano particles in the polymer by a solution supersaturation method to obtain a solid sol;
s3, preparing an intelligent window foil: and uniformly coating the solid solution glue solution on a glass substrate by using a coating method, and drying and demolding to obtain the intelligent window foil capable of adapting to the illumination intensity.
7. The method for preparing the intelligent window foil capable of adapting to illumination intensity according to claim 6, wherein the method comprises the following steps: in the step S1, the first solvent is N, N-dimethylformamide, the concentration of the photochromic inorganic nanoparticle precursor in the sol is 0.1-0.3 g/mL, the concentration of the catalyst in the sol is 0.02-0.03 g/mL, and the stirring time is 1-3 h;
in step S2, the second solvent is dichloroethane, and the concentration of the polymer in the second solvent is: 0.2 to 0.6g/mL.
8. The application of the intelligent window foil preparation method capable of adapting to illumination intensity according to any one of claims 1-7, which is characterized in that: the intelligent window foil is used for adjusting the transmittance of sunlight.
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| PCT/CN2022/104508 WO2024007275A1 (en) | 2022-07-05 | 2022-07-08 | Smart window foil self-adaptive to illumination intensity, and preparation method therefor and use thereof |
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| JP4289023B2 (en) * | 2003-05-26 | 2009-07-01 | 東亞合成株式会社 | Thermochromic material and thermochromic film or thermochromic glass using the same |
| JP4507066B2 (en) * | 2004-02-18 | 2010-07-21 | 多木化学株式会社 | Tungsten oxide-containing titanium oxide sol, production method thereof, coating agent and optical functional body |
| CN101024742B (en) * | 2006-02-21 | 2010-05-12 | 中国科学院化学研究所 | Nano coating with photochromic and sunlight control characteristics, its preparing method and use |
| JP5775248B2 (en) * | 2008-03-21 | 2015-09-09 | 国立大学法人 東京大学 | Photocatalyst material, organic matter decomposition method, interior member, air cleaning device, oxidizer manufacturing device |
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| CN113861468B (en) * | 2021-10-11 | 2024-01-23 | 中国科学技术大学先进技术研究院 | Preparation method of photochromic tungsten oxide film and photochromic product |
| CN116162268A (en) * | 2022-12-22 | 2023-05-26 | 深圳市国华光电科技有限公司 | Preparation method and application of photochromic film |
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