CN113387596A - Wear-resistant super-hydrophobic photovoltaic glass and preparation method thereof - Google Patents
Wear-resistant super-hydrophobic photovoltaic glass and preparation method thereof Download PDFInfo
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- CN113387596A CN113387596A CN202110882250.2A CN202110882250A CN113387596A CN 113387596 A CN113387596 A CN 113387596A CN 202110882250 A CN202110882250 A CN 202110882250A CN 113387596 A CN113387596 A CN 113387596A
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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
- C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
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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
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/213—SiO2
Abstract
Discloses a preparation method of wear-resistant super-hydrophobic photovoltaic glass, which comprises the following steps: acid-catalyzed nano SiO2Sol and base catalyzed nano SiO2Mixing the sol to form an antireflection film coating composition; adopting a dipping and pulling method to form SiO on the surface of the photovoltaic glass2An antireflection film; obtaining a multilayer PAH/silicate self-assembled film; vapor deposition forms a polyfluoro hydrophobic film. Also discloses a product obtained by the preparation method. The product has high light transmittance; meanwhile, the composite material has better mechanical property and super-hydrophobicity.
Description
Technical Field
The invention relates to wear-resistant super-hydrophobic photovoltaic glass and a preparation method thereof, and belongs to the technical field of photovoltaic glass.
Background
The photovoltaic industry association points out in published photovoltaic industry reports that photovoltaic glass with characteristics of dust prevention, pollution prevention, easy cleaning and the like has become one of the key points of attention in the industry. Therefore, further reducing the reflection loss of the surface of the photovoltaic glass, improving the light absorption rate of the photovoltaic cell, effectively reducing the manual cleaning cost of the photovoltaic module, and finding a high-transmittance antireflection film with a certain self-cleaning function is the most urgent need at present.
Surfaces with a self-cleaning function at the same time have the special property of not being wetted by water droplets, since the contact angle of a water droplet on the surface of the material is greater than 150 °. Similarly, in nature, lotus leaves, water striders, rice, and the like have surfaces with a self-cleaning function in nature. The research finds that the surface of the material with the self-cleaning function usually has super-hydrophobicity; further research shows that the super-hydrophobicity of the material surface is determined by the multi-layered micro-nano structure and the lower surface free energy. On one hand, due to the fact that the multi-level micro-nano structure exists on the surface, after water drops drop on the surface of the material, air exists between the water drops and the rough surface, the original solid-liquid interface is replaced by the solid-gas-liquid interface to a great extent, and therefore the interaction between the water drops and the surface of the material is reduced. On the other hand, on the surface of the material, there are generally substances with low surface free energy. The presence of these substances also makes it less likely that water droplets will wet out on the surface of the material.
Chinese patent CN107383949B discloses a preparation method of a wear-resistant self-cleaning photovoltaic glass antireflection hydrophobic coating liquid, which comprises the following steps: s1, dissolving perfluoroalkyl silane and tetraethyl orthosilicate in an organic solvent, adding an acid catalyst for hydrolysis, and removing the acid catalyst to obtain an acid catalytic reaction system; s2, dissolving perfluoroalkyl silane and tetraethyl orthosilicate in an organic solvent, adding an alkali catalyst for hydrolysis, removing the alkali catalyst, and aging to obtain an alkali catalytic reaction system; the organic solvent is the same as the organic solvent in step S1; s3, mixing the acid catalytic reaction system in the step S1 and the alkali catalytic reaction system in the step S2, and stirring uniformly to obtain the wear-resistant self-cleaning photovoltaic glass antireflection hydrophobic coating liquid. Spraying the anti-reflection hydrophobic coating liquid on the ultra-white glass, and curing at normal temperature. The contact angle of the obtained self-cleaning photovoltaic glass antireflection hydrophobic coating is 121-128 degrees, and the transmittance is 95.25-96.55 percent.
Chinese patent application CN107216044A discloses a nano antifouling coating liquid, which comprises the following raw materials: ethyl orthosilicate, organic modifier, deionized water, organic solvent and catalyst; the raw materials comprise the following components in percentage by weight: by weight, 100 parts of ethyl orthosilicate, 0-15 parts of organic modifier, 8-60 parts of deionized water, 0.5-15 parts of organic solvent and 0-12 parts of catalyst. After the nano antifouling coating liquid is coated on the surface of a photovoltaic glass substrate, a firm colorless, tasteless, smooth, transparent and about dozens of nanometers thick nano antifouling coating with excellent water-proof, oil-proof, antifouling and other characteristics similar to the lotus leaf surface can be formed on the surface of the photovoltaic glass substrate in a self-assembly mode. The antifouling coating of this nanometer isolates polar group such as most silicon hydroxyl in the photovoltaic glass substrate with external, and the difficult deposition of ash of photovoltaic power generation panel to certain angle slope is at nanometer coating protection lower surface to reduce the degree of difficulty and the frequency to the clean operation of photovoltaic power generation panel, reduced photovoltaic power plant operation maintenance cost, improved photovoltaic power generation's yield.
However, the hydrophobic properties of the above antireflection film are still unsatisfactory; meanwhile, there is still room for improvement in light transmittance and mechanical stability of the formed antireflection film.
Therefore, the above-mentioned defects of the prior art are still overcome, and a wear-resistant super-hydrophobic photovoltaic glass and a preparation method thereof are provided.
Disclosure of Invention
The invention aims to provide wear-resistant super-hydrophobic photovoltaic glass and a preparation method thereof.
In order to achieve the above object, in one aspect, the present invention provides a method for preparing a wear-resistant super-hydrophobic photovoltaic glass, comprising:
mixing Tetraethoxysilane (TEOS), absolute ethyl alcohol, deionized water and HCl, and aging to form acid-catalyzed nano SiO2Sol;
is prepared from Tetraethoxysilane (TEOS), absolute ethyl alcohol, deionized water and NH3·H2Mixing O, aging and refluxing to form base-catalyzed nano SiO2Sol;
acid catalyzed nano SiO2Sol and base catalyzed nano SiO2Mixing the sol to form an antireflection film coating composition;
a dipping and pulling method is adopted to form the anti-reflection film coating composition on the surface of the photovoltaic glass and the SiO is obtained by heat preservation at the temperature of 120-180 DEG C2Antireflection film, photovoltaic glass @ SiO obtained therefrom2An antireflection film;
photovoltaic glass @ SiO2Respectively soaking the antireflection film in a polyallylamine hydrochloride (PAH) aqueous solution and a sodium silicate aqueous solution for 5-30min, washing with water after each soaking, and drying by using nitrogen to obtain 1 layer of PAH/silicate self-assembled film on the surface of the antireflection film;
repeating the steps to obtain a multilayer PAH/silicate self-assembled film, thereby obtaining the photovoltaic glass @ SiO2Antireflection film @ (PAH/silicate self-assembled film);
the polyfluoro-substituted C6-14 alkyltrialkoxysilane reacts for 1-5h at the temperature of 100-140 ℃ to form a polyfluoro hydrophobic film by vapor depositionThe photovoltaic glass @ SiO is obtained2Antireflection film @ (PAH/silicate self-assembled film) @ polyfluoro hydrophobic film.
According to the preparation method, the molar ratio of Tetraethoxysilane (TEOS), absolute ethyl alcohol, deionized water and HCl is 1: (23-31): (2.8-4.4): (0.1-0.9).
Preferably, the molar ratio of tetraethyl orthosilicate (TEOS), absolute ethyl alcohol, deionized water and HCl is 1: (24-30): (3.0-4.2): (0.2-0.8).
More preferably, the molar ratio of Tetraethylorthosilicate (TEOS), absolute ethanol, deionized water and HCl is 1: (25-29): (3.2-4.0): (0.3-0.7).
Most preferably, the molar ratio of Tetraethylorthosilicate (TEOS), absolute ethanol, deionized water and HCl is 1: (26-28): (3.4-3.8): (0.4-0.6).
The preparation method provided by the invention is characterized in that the aging temperature is 20-40 ℃, and the aging time is 0.5-5.5 d.
Preferably, the aging temperature is 22-38 ℃ and the aging time is 1-5 d.
More preferably, the aging temperature is 25-35 ℃ and the aging time is 1.5-4.5 d.
Most preferably, the aging temperature is 28-32 ℃ and the aging time is 2-4 d.
In-base catalysis of nano SiO2When the sol is mixed, advantageously, anhydrous ethanol, deionized water and NH are first mixed3·H2O, and then adding Tetraethoxysilane (TEOS).
The preparation method comprises the steps of tetraethyl orthosilicate (TEOS), absolute ethyl alcohol, deionized water and NH3·H2The molar ratio of O is 1: (36-44): (1.6-2.4): (0.6-1).
Preferably, tetraethyl orthosilicate (TEOS), absolute ethyl alcohol, deionized water, NH3·H2The molar ratio of O is 1: (37-43): (1.7-2.3): (0.65-0.95).
More preferably, tetraethyl orthosilicate (TEOS), anhydrous ethanol, deionized water, NH3·H2The molar ratio of O is 1: (38-42): (1.8-2.2): (0.7-0.9).
Most preferably, Tetraethylorthosilicate (TEOS), anhydrous ethanol, deionized water, NH3·H2The molar ratio of O is 1: (39-41): (1.9-2.1): (0.75-0.85).
The preparation method provided by the invention is characterized in that the aging temperature is 20-40 ℃, and the aging time is 2-6 d; and/or the reflux temperature is 70-85 ℃, and the reflux time is 2-10 h.
Preferably, the aging temperature is 22-38 ℃, and the aging time is 2.5-5.5 d; and/or the reflux temperature is 72-85 ℃, and the reflux time is 3-9 h.
More preferably, the aging temperature is 25-35 ℃ and the aging time is 3-5 d; and/or the reflux temperature is 78-82 ℃, and the reflux time is 4-8 h.
Most preferably, the aging temperature is 28-32 ℃ and the aging time is 3.5-4.5 d; and/or the reflux temperature is 79-81 ℃, and the reflux time is 5-7 h.
According to the preparation method, the acid catalyzes the nano SiO2Sol and the base-catalyzed nano SiO2The volume ratio of the sol is 1: (1.5-4.5).
Preferably, the acid catalyzes nano SiO2Sol and the base-catalyzed nano SiO2The volume ratio of the sol is 1: (2-4).
More preferably, the acid catalyzes the nano SiO2Sol and the base-catalyzed nano SiO2The volume ratio of the sol is 1: (2.5-3.5).
Most preferably, the acid catalyzes the nano-SiO2Sol and the base-catalyzed nano SiO2The volume ratio of the sol is 1: 3.
the preparation method according to the present invention, wherein the SiO2The average thickness of the antireflection film is 80 to 160 nm.
Preferably, the SiO2The average thickness of the antireflection film is 90 to 150 nm.
More preferably, the SiO2The average thickness of the antireflection film is 100-140 nm.
Most preferably, the SiO2Average thickness of antireflection filmIs 110-130 nm.
The preparation method provided by the invention is characterized in that the body of the photovoltaic glass is selected from K9 photovoltaic glass.
In the invention, the K9 photovoltaic glass comprises the following components: SiO 22＝69.13％，B2O3＝10.75％，BaO＝3.07％，Na2O＝10.40％，K2O＝6.29％，As2O3＝0.36％。
The preparation method provided by the invention is characterized in that the pulling speed of the dipping pulling method is 80-120 mm/min.
Preferably, the pulling speed of the dipping pulling method is 85-115 mm/min.
More preferably, the pulling speed of the dip-pulling method is 90-110 mm/min.
Most preferably, the dipping and pulling method has a pulling speed of 95-105 mm/min.
The preparation method of the invention is characterized in that the average molecular weight Mw of the polyallylamine hydrochloride is 15000-90000 daltons.
Preferably, the polyallylamine hydrochloride has an average molecular weight Mw of 30000 and 80000 daltons.
More preferably, the polyallylamine hydrochloride has an average molecular weight Mw of 45000-70000 daltons.
The preparation method of the invention, wherein the concentration of the polyallylamine hydrochloride aqueous solution is 1.0 mg/mL; the pH value is 3.0-5.0.
Preferably, the polyallylamine hydrochloride aqueous solution has a concentration of 1.0 mg/mL; the pH value is 3.2-4.8.
More preferably, the polyallylamine hydrochloride aqueous solution has a concentration of 1.0 mg/mL; the pH value is 3.5-4.5.
Most preferably, the concentration of the polyallylamine hydrochloride aqueous solution is 0.9-1.1 mg/mL; the pH value is 3.8-4.2.
The preparation method of the invention is characterized in that the concentration of the silicate aqueous solution is 0.10-0.30 mg/mL; the pH value is 10.0-12.0.
Preferably, the concentration of the silicate aqueous solution is 0.12-0.28 mg/mL; the pH value is 10.2-11.8.
More preferably, the concentration of the aqueous silicate solution is 0.15-0.25 mg/mL; the pH value is 10.5-11.5.
Most preferably, the concentration of the aqueous silicate solution is 0.18-0.22 mg/mL; the pH value is 10.8-11.2.
According to the preparation method, the number of the PAH/silicate self-assembled film layers is 2-6.
Preferably, the number of layers of the PAH/silicate self-assembled film is 3-5.
In the invention, the two steps of soaking in the polyallylamine hydrochloride aqueous solution and the sodium silicate aqueous solution each time are summed into one period, and 1 layer of PAH/silicate self-assembled film is obtained on the surface of the antireflection film.
Advantageously, after the reaction is complete, it is removed; drying the mixture at the temperature of 140 ℃ and 160 ℃ for 1-5h to remove the unreacted polyfluoro-substituted C6-14 alkyl trialkoxysilane.
The preparation method is characterized in that the polyfluoro-substituted C6-14 alkyl trialkoxysilane is selected from polyfluoro-substituted C6-10 alkyl trialkoxysilanes.
In a specific embodiment, the polyfluoro-substituted C6-14 alkyltrialkoxysilane is selected from the group consisting of tridecafluorooctyltriethoxysilane (POTS).
In another aspect, the invention provides wear-resistant super-hydrophobic photovoltaic glass which is characterized by being obtained by the preparation method.
The inventors have found, in one aspect, that the aforementioned photovoltaic glass @ SiO according to the invention2The antireflection film @ (PAH/silicate self-assembled film) @ polyfluoro hydrophobic film not only improves the average light transmittance of the photovoltaic glass, but also obtains a multi-layered micro-nano structure and lower surface free energy on the surface through the structural design of a multilayer film, thereby reducing the contact angle and the rolling angle; and thus self-cleaning properties are obtained. On the other hand, SiO of photovoltaic glass2The antireflection film is prepared by catalyzing nano SiO with acid2Sol and base catalyzed nano SiO2The sol is mixed, has the technical advantages of both the sol and the sol, and not only has better performanceHigh light transmittance; meanwhile, the wear-resistant rubber has better mechanical properties, particularly wear resistance.
Detailed Description
The invention will be further illustrated with reference to specific embodiments.
It should be understood that the detailed description of the invention is merely illustrative of the spirit and principles of the invention and is not intended to limit the scope of the invention. Furthermore, it should be understood that various changes, substitutions, deletions, modifications or adjustments may be made by those skilled in the art after reading the disclosure of the present invention, and such equivalents are also within the scope of the invention as defined in the appended claims.
In the present invention, superhydrophobic means that a contact angle of a water droplet on a solid surface is 150 ° or more.
Example 1
Tetraethoxysilane (TEOS), absolute ethyl alcohol, deionized water and HCl are mixed and stirred for 2 hours, and the mixture is aged to form acid-catalyzed nano SiO2And (3) sol. Wherein the molar ratio of Tetraethoxysilane (TEOS), absolute ethyl alcohol, deionized water and HCl is 1: 27: 3.6: 0.5. then aging is carried out; the aging temperature is 30 ℃, the aging time is 3d, and the acid-catalyzed nano SiO is obtained2And (3) sol.
Firstly, absolute ethyl alcohol, deionized water and NH3·H2And O, adding Tetraethoxysilane (TEOS), mixing and stirring for 2 hours. Wherein, tetraethyl orthosilicate (TEOS), absolute ethyl alcohol, deionized water and NH3·H2The molar ratio of O is 1: 40: 2: 0.8. then aging is carried out; the aging temperature is 30 ℃ and the aging time is 4 d. Refluxing after aging at 80 deg.C for 6h to obtain base-catalyzed nanometer SiO2And (3) sol.
According to the volume ratio of 1: 3, catalyzing the acid with nano SiO2Sol and the base-catalyzed nano SiO2And (4) uniformly mixing the sol. The above sol was filtered using a 0.22 μm PVDF microfiltration membrane.
Adopting a dip-coating method to coat cleaned K9 photovoltaic glass (40 multiplied by 20 multiplied by 1 mm)3(ii) a Comprises the following components: SiO 22＝69.13％，B2O3＝10.75％，BaO＝3.07％，Na2O＝10.40％，K2O＝6.29％，As2O30.36%) was coated at a constant speed of 100 mm/min. Keeping the temperature of the film at 150 ℃ for 12h, and naturally cooling to room temperature to obtain the photovoltaic glass coated with the antireflection film, namely photovoltaic glass @ SiO2An antireflection film.
SiO2The average thickness of the antireflection film was 128.9 ± 7.2 nm.
Soaking the photovoltaic glass coated with the antireflection film in 1.0mg/mL polyallylamine hydrochloride (PAH; Mw: 60000 Dalton) water solution with the pH value of 4.0 for 20 min; taking out, washing with deionized water for 3 times, each time for 1min, and drying with nitrogen; then soaking the mixture in 0.2mg/mL sodium silicate aqueous solution with the pH value of 11.0 for 10 min; taking out, washing with deionized water for 3 times, each time for 1min, and blowing with nitrogen. The two steps are a period, and 1 layer of PAH/silicate self-assembled film is obtained on the surface of the antireflection film. Repeating for 3 cycles to obtain 4 layers of PAH/silicate self-assembled film on the surface of the antireflection film, namely the photovoltaic glass @ SiO2Antireflection film @ (PAH/silicate self-assembled film).
Photovoltaic glass @ SiO2The antireflection film @ (PAH/silicate self-assembled film) was placed in a jar, 0.2mL of tridecafluorooctyltriethoxysilane (POTS) was added dropwise, and the jar was sealed and reacted at 120 ℃ for 3 hours. Taking out after the reaction is finished; drying the glass at 145 ℃ for 2h to obtain the photovoltaic glass @ SiO2Antireflection film @ (PAH/silicate self-assembled film) @ polyfluoro hydrophobic film.
Performance characterization
And (3) testing light transmittance: the average light transmittance (%) of the antireflection film-coated photovoltaic glass was measured in the wavelength range of 380-800nm using a UV-visible spectrophotometer.
Super hydrophobicity test: photovoltaic glass @ SiO measured by contact angle tester2The contact angle and the roll angle of the antireflection film @ (PAH/silicate self-assembled film) @ polyfluoro hydrophobic film, and the water drop volume was 4 μ L.
The results are shown in Table 1.
TABLE 1
| Test specimen | Light transmittance | Contact angle | Roll angle |
| Example 1 | 94.2 | 150.9° | 5.7° |
And (3) testing the wear resistance: absorbent cotton dipped with dust and water is adopted to be coated on photovoltaic glass @ SiO2Antireflection film
The abrasion resistance of the film was evaluated by wiping the surface of a @ polyfluoro hydrophobic film 100 times back and forth at @ PAH/silicate self-assembled film, and measuring the average light transmittance (%) and contact angle of the film after washing and drying.
The results are shown in Table 2.
TABLE 2
| Test specimen | Light transmittance | Contact angle |
| Example 1 (after wiping) | 93.9 | 150.6 |
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of a wear-resistant super-hydrophobic antireflection film comprises the following steps:
mixing Tetraethoxysilane (TEOS), absolute ethyl alcohol, deionized water and HCl, and aging to form acid-catalyzed nano SiO2Sol;
is prepared from Tetraethoxysilane (TEOS), absolute ethyl alcohol, deionized water and NH3·H2Mixing O, aging and refluxing to form base-catalyzed nano SiO2Sol;
acid catalyzed nano SiO2Sol and base catalyzed nano SiO2Mixing the sol to form an antireflection film coating composition;
a dipping and pulling method is adopted to form the anti-reflection film coating composition on the surface of the photovoltaic glass and the SiO is obtained by heat preservation at the temperature of 120-180 DEG C2Antireflection film, photovoltaic glass @ SiO obtained therefrom2An antireflection film;
photovoltaic glass @ SiO2Respectively soaking the antireflection film in a polyallylamine hydrochloride (PAH) aqueous solution and a sodium silicate aqueous solution for 5-30min, washing with water after each soaking, and drying by using nitrogen to obtain 1 layer of PAH/silicate self-assembled film on the surface of the antireflection film;
repeating the steps to obtain a multilayer PAH/silicate self-assembled film, thereby obtaining the photovoltaic glass @ SiO2Antireflection film @ (PAH/silicate self-assembled film);
the polyfluoro-substituted C6-14 alkyl trialkoxysilane reacts for 1-5h at the temperature of 100-140 ℃ to form a polyfluoro hydrophobic film by vapor deposition, so that the photovoltaic glass @ SiO2Antireflection film @ (PAH/silicate self-assembled film) @ polyfluoro hydrophobic film.
2. The method of claim 1, wherein the molar ratio of tetraethyl orthosilicate (TEOS), absolute ethyl alcohol, deionized water and HCl is 1: (23-31): (2.8-4.4): (0.1-0.9).
3. The method of claim 1, wherein tetraethyl orthosilicate (TEOS), absolute ethanol, deionized water, NH3·H2The molar ratio of O is 1: (36-44): (1.6-2.4): (0.6-1).
4. The method of claim 1, wherein the acid catalyzes nano-SiO2Sol and the base-catalyzed nano SiO2The volume ratio of the sol is 1: (1.5-4.5).
5. The production method according to claim 1, wherein the SiO2The average thickness of the antireflection film is 80 to 160 nm.
6. The production method according to claim 1, wherein the dipping and pulling method has a pulling speed of 80 to 120 mm/min.
7. The process according to claim 1, wherein the polyallylamine hydrochloride has an average molecular weight Mw of 15000 and 90000 daltons.
8. The process of claim 1, wherein the concentration of the polyallylamine hydrochloride aqueous solution is 1.0 mg/mL; the pH value is 3.0-5.0; and/or the concentration of the silicate aqueous solution is 0.10-0.30 mg/mL; the pH value is 10.0-12.0.
9. The production method according to claim 1, wherein the number of layers of the PAH/silicate self-assembled film is 2 to 6.
10. An abrasion-resistant superhydrophobic antireflection film characterized by being obtained by the production method according to any one of claims 1 to 9.
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| CN115160942B (en) * | 2022-06-25 | 2024-02-27 | 苏州翎慧材料科技有限公司 | Optical product protective film and production method thereof |
| CN115555235A (en) * | 2022-10-28 | 2023-01-03 | 西南科技大学 | Preparation method of silicon dioxide antireflection film |
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