CN110606670A - Preparation method of broad-spectrum anti-reflection super-hydrophobic photovoltaic glass - Google Patents
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- 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
- 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
- C03C17/3417—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 all coatings being oxide coatings
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- C03—GLASS; MINERAL OR SLAG WOOL
- 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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/73—Anti-reflective coatings with specific characteristics
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- C03—GLASS; MINERAL OR SLAG WOOL
- 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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/76—Hydrophobic and oleophobic coatings
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- C03—GLASS; MINERAL OR SLAG WOOL
- 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- 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
- C03C2218/00—Methods for coating glass
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Abstract
The invention discloses a preparation method of broad-spectrum anti-reflection super-hydrophobic photovoltaic glass, which adopts a two-step method to prepare the broad-spectrum anti-reflection super-hydrophobic photovoltaic glass, firstly an alumina film with a porous structure is prepared on the glass, then silicon oxide nano-particles with the size of several nanometers to dozens of nanometers are filled in the porous structure, and heptadecafluorodecyltrimethoxysilane is utilized to reduce the surface energy of the silicon oxide nano-particles. The broad-spectrum anti-reflection super-hydrophobic film layer prepared on the surface of the photovoltaic glass has a double-scale structure, and the preparation method of the anti-reflection super-hydrophobic film layer with simple process and low cost is an effective solution for industrial application of the photovoltaic glass, curtain wall glass, automobile glass and the like.
Description
Technical Field
The invention belongs to the technical field of photovoltaics, and particularly relates to a preparation method of broad-spectrum anti-reflection super-hydrophobic photovoltaic glass.
Background
With the increasing prominence of the problems of resource unsustainability, environmental pollution and the like, as solar energy has the characteristics of rich resources, wide distribution, environmental friendliness and the like, photovoltaic power generation has become a main choice for new energy development in the future, and is a new industry with global general attention and key development. The cost of photovoltaic power generation depends on the photoelectric conversion efficiency of the photovoltaic module, and the higher the efficiency of the module, the lower the power generation cost. The efficiency of the solar cell is a decisive factor of the module efficiency, and the maximum conversion efficiency of the crystalline silicon cell reaches 26.7 percent at present and reachesVery close to its theoretical conversion of 29.3%, there has been less and less room to further increase cell efficiency. Because the photovoltaic module is installed outdoors, dust is easily accumulated on the surface of the photovoltaic glass of the protection module, the light transmittance of the glass is greatly reduced, and the conversion efficiency of the photovoltaic module is finally reduced. Researches show that the photovoltaic module is arranged on a dust deposition density of 0.1-10 g/m2After 5 months the efficiency of the module dropped by 30%. In order to optimize the output of the photovoltaic module, the module should be cleaned regularly, which, however, will increase the cost of photovoltaic power generation. In addition, the optical transmittance of the photovoltaic glass has a great influence on the efficiency of the module, the current mainstream photovoltaic glass is mainly low-iron tempered suede glass, the optical transmittance in the wavelength range of 400-1100 nm reaches 92%, and the transmittance still has 8% of promotion space. Therefore, by improving the optical transmittance of the photovoltaic glass and the cleanliness during long-term outdoor operation of the photovoltaic module, the development of a crystalline silicon cell with higher conversion rate is easier and the cost is much lower.
The reflection of the photovoltaic glass to sunlight is reduced, and two methods can be realized. In the first method, a single layer or a multilayer film with a certain thickness is coated on the surface of the glass, and the reflected light is eliminated by utilizing the principle of light interference. Because the sunlight is the compound light with wide frequency spectrum, the single-layer antireflection film only has the effect of complete antireflection on the monochromatic light with a certain specific wavelength in the sunlight and only has partial antireflection effect on the light with other wavelengths. Although the antireflection effect can be improved by the multilayer plating technique, the cost is high. The second method is to prepare a film having a nanostructure on the surface of glass, which has superior anti-reflective properties to a multi-layer anti-reflective film, has superior anti-reflective properties over a wide angle and a wide spectrum, and can reduce the reflectance to 1% over a wide wavelength.
Because the gaps between the nano-clusters (such as nanowires, nanorods, nano-columns and the like) are much smaller than the wavelengths of visible light and infrared light, the nano-structure film layer can be equivalent to a single homogeneous film with the refractive index between air and the nano-cluster material, the refractive index is reduced along with the increase of the porosity, light enters the equivalent refraction field, the light resonance disappears, and no diffraction is generated. The film with the nano structure has the characteristic of gradual change of the refractive index, so that the Fresnel reflection capability at the interface of the film and air can be fundamentally eliminated, and the film has the antireflection characteristic of wide waveband and wide angle. This anti-reflective property of the nanostructures depends on the size of the nanostructures, and gradually degrades as the periodic size of the structure gradually increases. When the size of the nanostructure is close to or larger than the wavelength of incident light, that is, a so-called textured structure, although the antireflection performance induced by the refractive index gradation characteristic disappears, the incident light may be reflected on the surface of the substrate many times, increasing the absorption of light, thereby reducing the surface reflection.
The self-cleaning function of lotus leaf surfaces is well known and is due to their super-hydrophobic nature. A large number of micron-sized waxy mastoid structures are distributed on the surface of the lotus leaf, the waxy substance has low surface energy, each mastoid surface is composed of a nano-scale fibrous structure to form a micron-nano composite structure (micro-nano structure for short), and the micro-nano structure is a key factor for forming a super-hydrophobic surface. The special structure can effectively form an air layer, greatly reduces the contact area between the lotus leaf surface and water drops, dust and the like, reduces the rolling angle, ensures that water drops easily roll off on the lotus leaf surface, takes away the dust on the lotus leaf surface, and plays a role in automatically cleaning the lotus leaf surface. The preparation method of the artificial super-hydrophobic surface structure generally comprises the steps of firstly forming a micro-nano structure on the surface and then carrying out low surface energy modification. The low surface energy is a prerequisite for forming the super-hydrophobic surface, and the surface micro-nano structure is a determining factor for the super-hydrophobic performance.
The low surface energy film with the micro-nano structure is constructed on the surface of the photovoltaic glass, so that the reflection of sunlight on the surface of the glass can be greatly reduced, the optical transmittance of the glass is increased, a super-hydrophobic surface can be formed, the cleanliness of the surface of the glass can be kept under the washing of rainwater, and the self-cleaning function is realized. The anti-reflection effect of the surface of the nano structure on sunlight is better than that of the micro structure, the surface of the micro-nano composite structure has better hydrophobic property, but the optical transmittance of the glass can be adversely affected by the existence of the micro structure, so that the high light transmittance and the super-hydrophobic property are contradictory.
At present, two approaches are mainly used for preparing the surface of the anti-emission super-hydrophobic glass, one is to coat inorganic oxides such as silicon dioxide or titanium dioxide on the surface of the glass, and the other is to directly form a micron-nano composite structure on the surface of the glass. The first method is that the durability of the surface is weak because the porous structure formed by the accumulation of nanoparticles imparts the super-hydrophobic surface anti-reflection property to the surface. The second method is to form a porous structure on the surface of the glass by a wet or dry etching process, which is excellent in hydrophobic property but poor in optical transmittance. How to obtain the broad-spectrum anti-reflection super-hydrophobic photovoltaic glass by improving the preparation method of the surface microstructure and optimizing the surface structure is a difficult problem which is urgently needed to be solved by the photovoltaic industry at present.
The alumina film has strong binding force with the glass substrate, and has excellent performances of high optical transmittance, scratch resistance, wear resistance and the like. Therefore, in the present invention, alumina is utilized as a modifying material for transparent hydrophobic photovoltaic glass. In order to improve the surface roughness of the alumina film, a low-temperature hydrothermal treatment is utilized to obtain a micron-nano composite porous structure. In order to increase the optical transmittance of the glass, nanoparticles such as silicon oxide, titanium oxide, and zinc oxide are filled in the porous structure. Finally, in order to reduce the surface energy, organic polymers such as alkoxysilates, alkoxy polymers and fluorides can be used for modification treatment, and finally the broad-spectrum anti-reflection super-hydrophobic photovoltaic glass is obtained.
Disclosure of Invention
The invention aims to provide a preparation method of broad-spectrum anti-reflection super-hydrophobic photovoltaic glass.
The general idea of the invention is as follows: the method adopts a two-step method to prepare the broad-spectrum anti-reflection super-hydrophobic photovoltaic glass, and firstly, the alumina (Al) with a porous structure is prepared on the glass2O3) A thin film, and then filling silicon oxide (SiO) having a size of several to several tens of nanometers in the porous structure2) And reducing the surface energy of the silicon oxide nanoparticles by using heptadecafluorodecyltrimethoxysilane.
Specifically, the invention adopts the following technical scheme:
a preparation method of broad-spectrum anti-reflection super-hydrophobic photovoltaic glass comprises the following steps:
1) cleaning and hydroxylating a glass substrate: immersing the cleaned glass substrate into a mixed solution of concentrated sulfuric acid and hydrogen peroxide, wherein the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 4:9, performing ultrasonic oscillation for 1-3 hours at normal temperature, taking out, cleaning again and drying;
2) preparing alumina sol: mixing aluminum trichloride hexahydrate and absolute ethyl alcohol according to a molar ratio of 1: 20-30, fully and uniformly stirring, slowly dripping acetylacetone (the molar ratio of the acetylacetone to the aluminum trichloride hexahydrate is 3:1) into the mixed solution, stirring for 1-2 hours, adding an anionic surfactant (the mole number of the anionic surfactant is 0.1-1.0% of that of the aluminum trichloride hexahydrate), and stirring for 1-2 hours in a water bath at 65 ℃ to obtain uniformly dispersed alumina sol;
3) preparing a porous alumina film: coating the alumina sol obtained in the step 2) on the glass substrate obtained in the step 1) by adopting a spin coating method, wherein the thickness is controlled within the range of 150-250 micrometers; after coating, putting the substrate into a muffle furnace for low-temperature annealing, wherein the annealing temperature is 400-450 ℃, and the annealing time is 60-90 min; cleaning and blow-drying after annealing;
4) preparing nano silica sol: under the conditions of constant-temperature water bath at 60 ℃ and magnetic stirring, slowly dissolving a proper amount of L-lysine in a mixed solution of isopropanol and deionized water, slowly dropwise adding ethyl orthosilicate into the mixed solution, stirring for reaction for 2-3 hours, and standing for 10 hours; in the solution, the molar ratio of the ethyl orthosilicate to the L-lysine to the isopropanol to the deionized water is 1: 0.01-0.03: 2.5: 150-300;
5) preparing fluorine modified nano silica sol: adding heptadecafluorodecyltrimethoxysilane and ethanol into the nano silica sol obtained in the step 4), and magnetically stirring for 2 hours in a constant-temperature water bath environment at the temperature of 60 ℃; wherein the molar ratio of the ethyl orthosilicate to the heptadecafluorodecyltrimethoxysilane to the ethanol is 1: 1-3: 5-8;
6) coating the fluorine modified nano silica sol obtained in the step 5) on the glass substrate obtained in the step 3) by adopting a spin coating method, then drying the substrate in an electric heating oven at the temperature of 80 ℃ for 30min, and annealing the substrate in a muffle furnace at a low temperature for 2h, wherein the annealing temperature is 200 ℃.
The broad-spectrum anti-reflection super-hydrophobic film layer prepared on the surface of the photovoltaic glass has a double-scale structure. In the process of carrying out low-temperature hydrothermal treatment on the alumina film, a three-dimensional cross-linked network-shaped porous structure with nano holes is formed, and the silica nano particles are attached to the nano hole structure, so that the size of the hole structure is reduced, and the reflection of the surface is reduced. The average transmittance of the film layer in the wavelength range of 400-1100 nm is 96.44%, and the surface contact angle is 161.80. In addition, the film layer has stronger corrosion resistance and durability. The preparation method of the anti-reflection super-hydrophobic film layer with simple process and low cost is an effective solution for industrial application of photovoltaic glass, curtain wall glass, automobile glass and the like.
Drawings
The following detailed description is made with reference to the accompanying drawings and embodiments of the present invention
FIG. 1 is a circuit diagram of a preparation process of broad-spectrum anti-reflection super-hydrophobic photovoltaic glass;
fig. 2 is an optical transmittance of a broad spectrum antireflective superhydrophobic photovoltaic glass.
Detailed Description
1. Main experimental raw material and instrument and equipment
A glass substrate: 40mm multiplied by 0.2mm, and the visible light transmittance of the ultra-white float low-iron glass is 91 percent;
aluminum trichloride hexahydrate (AlCl)3·6H2O)：99％；
Acetylacetone (C)5H8O2)：99.5％；
Tetraethoxysilane (TEOS, C)8H20O4Si)：99％；
L-lysine (L-lysine): 98 percent of
Heptadecafluorodecyltrimethoxysilane (1H,1H,2H, 2H-Perfluorodecyltrimethylysilane): 97 percent;
sodium Dodecyl Benzene Sulfonate (DBS): 95 percent;
common chemical reagents such as sulfuric acid, hydrogen peroxide, absolute ethyl alcohol and isopropanol: analyzing and purifying;
deionized water: the resistivity is greater than 18.2M omega cm;
a magnetic stirrer, an electric heating oven, an ultrasonic cleaning machine, a muffle furnace, an electric heating constant-temperature water tank, a rotary coating instrument and the like;
a contact angle tester and an ultraviolet visible near-infrared spectrophotometer.
2. Glass substrate cleaning and hydroxylation treatment
In order to increase the hydrophilicity of the glass surface and enhance the bonding force between the alumina film and the glass substrate, surface hydroxylation treatment is required, and the specific method comprises the following steps:
firstly, ultrasonically cleaning by using a detergent solution for 30min, then repeatedly washing by using tap water until no bubbles exist, and repeatedly cleaning by using deionized water until the conductivity of water is close to that of the deionized water;
secondly, carrying out surface hydroxylation treatment, namely immersing the cleaned glass substrate into concentrated sulfuric acid and hydrogen peroxide at a volume mixing ratio of 4:9, carrying out ultrasonic oscillation at normal temperature for 1-3 h, taking out, repeatedly washing with deionized water, and drying with nitrogen for later use.
3. Preparation of alumina sol
Mixing aluminum trichloride hexahydrate and absolute ethyl alcohol according to a molar ratio of 1: 20-30, fully and uniformly stirring, slowly dripping acetylacetone (the molar ratio of the acetylacetone to the aluminum trichloride hexahydrate is 3:1) into the mixed solution, magnetically stirring for 1-2 hours, then adding a small amount of anionic surfactant, namely sodium dodecyl benzene sulfonate (the molar number is 0.1-1.0% of the aluminum trichloride hexahydrate), stirring for 1-2 hours under a water bath condition of 65 ℃, and finally obtaining the uniformly dispersed alumina sol.
4. Preparation of porous alumina film
And coating the prepared alumina sol on a glass substrate with the surface subjected to hydroxylation treatment by adopting a spin coating method, and adjusting the thickness of the spin coating liquid by using the rotating speed and time of a rotating disc, wherein the thickness is controlled within the range of 150-250 mu m. And after coating, putting the substrate into a muffle furnace for low-temperature annealing, wherein the annealing temperature is 400-450 ℃, and the annealing time is 60-90 min. And after the annealing is finished, naturally cooling the furnace to room temperature, taking out the glass substrate, then placing the glass substrate into deionized water at the temperature of 80-95 ℃ for hydrothermal treatment for 15-25 min, washing with group ionized water after the hydrothermal treatment is finished, and drying with nitrogen.
5. Preparation of nano silica sol
Under the conditions of constant-temperature water bath at 60 ℃ and magnetic stirring, taking a proper amount of L-lysine to slowly dissolve in a mixed solution of isopropanol and deionized water, then slowly dropwise adding ethyl orthosilicate into the mixed solution, stirring for reaction for 2-3 h, and then standing for 10 h. In the solution, the molar ratio of the ethyl orthosilicate, the L-lysine, the isopropanol and the deionized water is 1: 0.01-0.03: 2.5: 150-300. The silicon oxide nanospheres obtained by the method have the particle size distribution within the range of 5-30 nm, and the particle size of the nanospheres can be regulated and controlled by changing the amount of reactants such as ethyl orthosilicate and L-lysine, for example, the amount of L-lysine is increased, the particle size is reduced, the amount of ethyl orthosilicate is increased, and the particle size is increased.
6. Preparation of fluorine modified nano silica sol
Adding a proper amount of heptadecafluorodecyltrimethoxysilane and ethanol into the nano silica sol, and magnetically stirring for 2 hours in a constant-temperature water bath environment at the temperature of 60 ℃. Under the process condition, the molar ratio of the ethyl orthosilicate to the heptadecafluorodecyltrimethoxysilane to the ethanol is 1: 1-3: 5-8.
7. Preparation of broad-spectrum anti-reflection super-hydrophobic photovoltaic glass
Coating fluorine modified nano silica sol on a glass substrate with a porous alumina film on the surface by adopting a spin-coating method, then drying the substrate in an electric heating oven at the temperature of 80 ℃ for 30min, and annealing the substrate in a muffle furnace at a low temperature for 2h, wherein the annealing temperature is 200 ℃.
8. Performance testing
Tests of an electron scanning microscope (SEM) show that the glass substrate treated by the process forms a three-dimensional cross-linked network-shaped porous structure with nano holes (the diameter of the nano holes is 200-600 nm) in the process of carrying out low-temperature hydrothermal treatment on an alumina film, and silica nano particles with the average particle size of 15nm are attached to the nano hole structure, so that the size of the hole structure is reduced, and a double-scale structure is formed. An ultraviolet visible near-infrared spectrophotometer is adopted to test the optical transmittance of the glass substrate, the average transmittance is 96.44 percent in the wavelength range of 400-1100 nm, and the highest transmittance is 98.2 percent, as shown in figure 2. The wettability of the obtained super-hydrophobic surface was tested by 5 μ l of liquid drop under room temperature environment, and when the water drop was left standing for 5s after falling on the surface, the contact angle of the glass surface was 161.8 °. After the glass substrate is soaked in an acid solution (hydrochloric acid solution with the pH of 4.0) and an alkaline solution (sodium hydroxide solution with the pH of 10) for 48 hours, the reduction of the light transmittance after corrosion is less than 1.0%. In addition, the surface film layer passed the 5H pencil hardness test.
Claims (1)
1. A preparation method of broad-spectrum anti-reflection super-hydrophobic photovoltaic glass is characterized by comprising the following steps: the method comprises the following steps:
1) cleaning and hydroxylating a glass substrate: immersing the cleaned glass substrate into a mixed solution of concentrated sulfuric acid and hydrogen peroxide, wherein the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 4:9, performing ultrasonic oscillation for 1-3 hours at normal temperature, taking out, cleaning again and drying;
2) preparing alumina sol: mixing aluminum trichloride hexahydrate and absolute ethyl alcohol according to a molar ratio of 1: 20-30, fully and uniformly stirring, slowly dripping acetylacetone (the molar ratio of the acetylacetone to the aluminum trichloride hexahydrate is 3:1) into the mixed solution, stirring for 1-2 hours, adding an anionic surfactant (the mole number of the anionic surfactant is 0.1-1.0% of that of the aluminum trichloride hexahydrate), and stirring for 1-2 hours in a water bath at 65 ℃ to obtain uniformly dispersed alumina sol;
3) preparing a porous alumina film: coating the alumina sol obtained in the step 2) on the glass substrate obtained in the step 1) by adopting a spin coating method, wherein the thickness is controlled within the range of 150-250 micrometers; after coating, putting the substrate into a muffle furnace for low-temperature annealing, wherein the annealing temperature is 400-450 ℃, and the annealing time is 60-90 min; cleaning and blow-drying after annealing;
4) preparing nano silica sol: under the conditions of constant-temperature water bath at 60 ℃ and magnetic stirring, slowly dissolving a proper amount of L-lysine in a mixed solution of isopropanol and deionized water, slowly dropwise adding ethyl orthosilicate into the mixed solution, stirring for reaction for 2-3 hours, and standing for 10 hours; in the solution, the molar ratio of the ethyl orthosilicate to the L-lysine to the isopropanol to the deionized water is 1: 0.01-0.03: 2.5: 150-300;
5) preparing fluorine modified nano silica sol: adding heptadecafluorodecyltrimethoxysilane and ethanol into the nano silica sol obtained in the step 4), and magnetically stirring for 2 hours in a constant-temperature water bath environment at the temperature of 60 ℃; wherein the molar ratio of the ethyl orthosilicate to the heptadecafluorodecyltrimethoxysilane to the ethanol is 1: 1-3: 5-8;
6) coating the fluorine modified nano silica sol obtained in the step 5) on the glass substrate obtained in the step 3) by adopting a spin coating method, then drying the substrate in an electric heating oven at the temperature of 80 ℃ for 30min, and annealing the substrate in a muffle furnace at a low temperature for 2h, wherein the annealing temperature is 200 ℃.
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| CN114436543A (en) * | 2022-01-07 | 2022-05-06 | 常州亚玛顿股份有限公司 | Coated glass for photovoltaic module and preparation method thereof |
| CN114436543B (en) * | 2022-01-07 | 2023-06-02 | 常州亚玛顿股份有限公司 | Coated glass for photovoltaic module and preparation method thereof |
| CN115340674A (en) * | 2022-08-17 | 2022-11-15 | 广东工业大学 | Silicone resin for rapid 3D printing and preparation method and application thereof |
| CN115340674B (en) * | 2022-08-17 | 2023-09-29 | 广东工业大学 | Silicon resin for rapid 3D printing and preparation method and application thereof |
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