CN115073016B - Preparation method of high-transmittance superhydrophobic antireflection film - Google Patents
Preparation method of high-transmittance superhydrophobic antireflection film Download PDFInfo
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- CN115073016B CN115073016B CN202210668998.7A CN202210668998A CN115073016B CN 115073016 B CN115073016 B CN 115073016B CN 202210668998 A CN202210668998 A CN 202210668998A CN 115073016 B CN115073016 B CN 115073016B
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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
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
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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
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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
- C03C2217/70—Properties of coatings
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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
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention discloses a preparation method of a high-transmittance superhydrophobic antireflection film, which relates to the technical field of optical film materials, and the preparation method comprises the steps of preparing SiO (silicon dioxide) by taking tetraethoxysilane as a precursor, water as a reactant, absolute ethyl alcohol as a solvent and ammonia water as a catalyst 2 Sol; after the sol is aged completely, adding hexamethyldisilazane into the sol to carry out hydrophobic modification on the sol; finally, a single-layer antireflection film is plated on two sides of the glass by adopting a dipping-pulling method. The high-transmittance superhydrophobic antireflection film with the transmittance larger than 99.8% and the water contact angle larger than 160 DEG is prepared by the method; the preparation method of the antireflection film has the characteristics of simple technical process, less required equipment, no need of high-temperature treatment, low preparation cost, convenient operation, easy realization of industrialization and the like.
Description
Technical field:
the invention relates to the technical field of optical film materials, in particular to a preparation method of a high-transmittance super-hydrophobic antireflection film.
The background technology is as follows:
the antireflection film is also called an antireflection film, is a film for reducing the surface reflection of an optical element and increasing the transmittance of light, and is widely applied to the fields of solar cells, solar heat collection tubes, high-energy laser systems and the like at present. The preparation method of the common antireflection film mainly comprises the following steps: phase separation, etching, bevel coating, layer-by-layer self-assembly and sol-gel. The sol-gel method for preparing the antireflection film has the advantages of simple operation, low cost, good uniformity of large-area film formation, independent adjustment of the microstructure and chemical composition of the film, and the like. SiO (SiO) 2 Is the most commonly used antireflection film material by sol-gel method, and SiO is prepared by the method 2 The antireflection film is formed by the film plating after the hydrolysis condensation of the alkali-catalyzed tetraethoxysilane 2 Film with nano particles randomly piled on substrate surface, particlesThe voids reduce the refractive index of the film such that the film refractive index is approximately 1.23 square root of the substrate refractive index and thus has a peak transmittance of about 100%. More importantly, the antireflection film prepared by the sol-gel method has a higher threshold value of laser damage resistance (two times of that of other methods such as a chemical deposition method) and is the only antireflection film applied to a high-energy laser system at present. But SiO prepared by sol-gel method 2 An antireflection film belongs to an inorganic film, siO 2 The surface of the nanoparticle contains a large amount of hydroxyl groups, so that water and pollutants in the surrounding environment are easily adsorbed, the transmittance of the film is reduced, and the practical application value of the film is limited. Therefore, in the practical use process of the antireflection film, the good environmental resistance is required to be considered.
By orientation to SiO 2 The anti-reflection film can effectively improve the environmental resistance of the film by introducing hydrophobic groups to replace hydroxyl groups on the surfaces of particles. The greater the hydrophobicity of the film surface, the better the environmental resistance of the film. When the surface of the film reaches a superhydrophobic state (contact angle greater than 150 ° and roll angle less than 5 °), the film will also exhibit good self-cleaning. The superhydrophobic self-cleaning property is mainly determined by hydrophobic groups on the surface of the film and the roughness of the surface of the film. According to the Wenzel formula, the greater the film surface roughness, the better the hydrophobicity of the film, but the higher surface roughness in turn exacerbates the scattering of the film surface and reduces the film transmittance. Since the transmittance and roughness are mutually exclusive, most of the currently reported superhydrophobic films have low transmittance, and the transmittance of some superhydrophobic films is even smaller than that of the substrate. Therefore, the surface roughness is required to be strictly controlled to obtain the film with ultra-high transmittance>99.8%) and superhydrophobic antireflection films. Xu Y et al (Applied optics 2005,44 (4)), 527-533 propose the use of hexamethyldisilazane for SiO 2 Modifying the sol to obtain SiO 2 The hydroxyl groups on the surface of the sol particles are replaced by methyl groups, so that super-hydrophobic SiO can be obtained 2 The film has low surface roughness and can not cause scattering. However, the introduction of hydrophobic groups reduces the capillary force during the sol film formation process, resulting in a decrease in the refractive index of the film. Zhang X et al (Advanced Functional Materials 2013,20,4361-4365) reported thatSuper-hydrophobic SiO obtained after modification by hexamethyldisilazane 2 The film refractive index would decrease from 1.23 to 1.13 initially, which would result in a peak transmittance decrease from 100% to 98.8%. Although the above is described for SiO by hexamethyldisilazane 2 The sol is modified to obtain a super-hydrophobic film with higher transmittance, but still has certain transmittance loss, and cannot meet the application in some fields, for example, the transmittance of an antireflection film required by a high-energy laser system is required to be more than 99.5%. Therefore, the film has ultra-high transmittance>99.8%) and superhydrophobic antireflection films remain technical challenges to be addressed.
The invention comprises the following steps:
in order to overcome the technical problems pointed out by the technical background, the invention provides a preparation method of a high-transmittance superhydrophobic antireflection film. Modification of SiO due to hexamethyldisilazane 2 The refractive index of the film obtained by the sol is reduced, and the invention proposes to change the initial SiO 2 The sol formula increases the water content, improves the refractive index of the film, and then modifies the sol by hexamethyldisilazane to reduce the refractive index, thus obtaining the film with the refractive index of 1.21-1.25. By the method, the film with the peak transmittance of more than 99.8% is obtained, and the superhydrophobicity of the film is maintained.
The technical problems to be solved by the invention are realized by adopting the following technical scheme:
the invention aims at providing a preparation method of a high-transmittance superhydrophobic antireflection film, which comprises the following steps:
(1) Sequentially adding absolute ethyl alcohol, deionized water, ammonia water and tetraethoxysilane into a reaction bottle, reacting at constant temperature, sealing and aging to obtain SiO 2 Sol;
(2) To the SiO produced in step (1) 2 Adding hexamethyldisilazane into the sol, reacting at constant temperature, sealing and aging to obtain hydrophobically modified SiO 2 Sol;
(3) Adopting a dipping-pulling method to prepare the hydrophobically modified SiO in the step (2) 2 The sol is plated on the surface of a glass substrate, and is dried at room temperature, so that the high-transmittance superhydrophobic antireflection film is finally obtained.
The molar ratio of the absolute ethyl alcohol to the deionized water to the ammonia water to the tetraethoxysilane in the step (1) is (30-40): 6-12): 0.15-0.18): 1.
The temperature of the constant temperature reaction in the step (1) is 25-30 ℃ and the time is 1-6h; the temperature of the sealing and aging is 25-30 ℃ and the time is 7-10 days.
The molar ratio of hexamethyldisilazane in step (2) to ethyl orthosilicate in step (1) (0.37-1.11): 1.
The temperature of the constant temperature reaction in the step (2) is 25-30 ℃ and the time is 1-6h; the temperature of the sealing and aging is 25-30 ℃ and the time is 5-10 days.
The speed of pulling the glass substrate out of the sol in the step (3) is 1000-6000 mu m/s.
The second purpose of the invention is to provide a high-transmittance superhydrophobic antireflection film prepared by the preparation method.
The thickness of the high-transmittance super-hydrophobic antireflection film is 81-183nm, and the refractive index is 1.21-1.25.
The peak transmittance of the high-transmittance super-hydrophobic antireflection film is greater than 99.8%, and the water contact angle is greater than 160 °.
The beneficial effects of the invention are as follows: the invention solves the problem that the existing hydrophobic antireflection film cannot have high transmittance and superhydrophobicity, and obtains the antireflection film with high transmittance and superhydrophobicity; the preparation method of the antireflection film provided by the invention has the characteristics of simple technical process, less required equipment, no need of high-temperature treatment, low preparation cost, convenience in operation, easiness in realization of industrialization and the like.
Description of the drawings:
FIG. 1 is a graph showing transmittance curves of antireflection films prepared in examples of the present invention and comparative examples;
fig. 2 is a schematic view showing water contact angles of the antireflection films prepared in the examples and the comparative examples of the present invention.
The specific embodiment is as follows:
in order that the manner in which the invention is practiced, features of the invention, as well as the manner in which it is attained and can be understood in detail, a more particular description of the invention, briefly summarized below, may be had by reference to embodiments, examples of embodiments, and the like.
Comparative example 1
(1) Sequentially adding absolute ethyl alcohol, deionized water, ammonia water and tetraethoxysilane into a reaction bottle according to a molar ratio of 38:4:0.17:1, reacting for 2 hours at a constant temperature of 25 ℃, and then aging for 7 days at a constant temperature of 25 ℃ in a sealing manner to obtain the standard SiO 2 And (3) sol.
(2) Immersing a glass substrate into a standard SiO 2 Coating film in sol at a lifting speed of 3000 mu m/s, and airing at room temperature.
The refractive index of the obtained antireflection film is 1.22, and the transmittance thereof at 519nm is 99.94%, as shown in fig. 1; the contact angle with water was 26 deg., as shown in figure 2.
Comparative example 2
(1) Sequentially adding absolute ethyl alcohol, deionized water, ammonia water and tetraethoxysilane into a reaction bottle according to a molar ratio of 38:16:0.17:1, reacting for 2 hours at a constant temperature of 25 ℃, and then sealing and aging for 7 days at the constant temperature of 25 ℃ to obtain the anhydrous SiO 2 And (3) sol.
(2) Immersing a glass substrate into a polyhydrated SiO 2 Coating film in sol at a lifting speed of 5000 μm/s, and airing at room temperature.
The refractive index of the obtained antireflection film was 1.30, and the transmittance thereof at 713nm was 99.41%, as shown in FIG. 1; the water contact angle was 11 °, as shown in fig. 2.
Comparative example 3
(1) Sequentially adding absolute ethyl alcohol, deionized water, ammonia water and tetraethoxysilane into a reaction bottle according to a molar ratio of 38:4:0.17:1, reacting for 2 hours at a constant temperature of 25 ℃, and then aging for 7 days at a constant temperature of 30 ℃ in a sealing manner to obtain SiO 2 And (3) sol.
(2) To SiO 2 Adding hexamethyldisilazane into the sol according to the mol ratio of hexamethyldisilazane to tetraethoxysilane of 0.37:1, reacting for 2 hours at the constant temperature of 25 ℃, and aging for 7 days at the constant temperature of 30 ℃ in a sealing way to obtain the hydrophobic modified SiO 2 And (3) sol.
(3) Immersing a glass substrate into hydrophobically modified SiO 2 Coating film in sol at a lifting speed of 3000 mu m/s, and airing at room temperature.
The refractive index of the obtained antireflection film is 1.13, and the transmittance of the antireflection film at 566nm is 98.85%, as shown in fig. 1; the water contact angle was 166 °, as shown in fig. 2.
Example 1
(1) Sequentially adding absolute ethyl alcohol, deionized water, ammonia water and tetraethoxysilane into a reaction bottle according to a molar ratio of 38:6:0.17:1, reacting for 2 hours at a constant temperature of 25 ℃, and then aging for 7 days at a constant temperature of 30 ℃ in a sealing manner to obtain SiO 2 And (3) sol.
(2) To SiO 2 Adding hexamethyldisilazane into the sol according to the mol ratio of hexamethyldisilazane to tetraethoxysilane of 0.37:1, reacting for 2 hours at the constant temperature of 25 ℃, and aging for 7 days at the constant temperature of 30 ℃ in a sealing way to obtain the hydrophobic modified SiO 2 And (3) sol.
(3) Immersing a glass substrate into hydrophobically modified SiO 2 Coating film in sol at a lifting speed of 1500 mu m/s, and airing at room temperature.
The refractive index of the obtained antireflection film is 1.23, and the transmittance of the antireflection film at 511nm is 99.94%, as shown in fig. 1; the water contact angle was 161 deg., as shown in figure 2.
Example 2
(1) Sequentially adding absolute ethyl alcohol, deionized water, ammonia water and tetraethoxysilane into a reaction bottle according to a molar ratio of 35:8:0.17:1, reacting for 2 hours at a constant temperature of 25 ℃, and then aging for 7 days at a constant temperature of 25 ℃ in a sealing manner to obtain SiO 2 And (3) sol.
(2) To SiO 2 Adding hexamethyldisilazane into the sol according to the mol ratio of hexamethyldisilazane to tetraethoxysilane of 0.64:1, reacting for 4h at 25 ℃ and ageing for 7 days at 25 ℃ in a sealing way, thus obtaining the hydrophobic modified SiO 2 And (3) sol.
(3) Immersing a glass substrate into hydrophobically modified SiO 2 Coating film in sol at the lifting speed of 4000 μm/s and airing at room temperature.
The refractive index of the obtained antireflection film is 1.21, and the transmittance of the antireflection film at 624nm is 99.85%, as shown in figure 1; the water contact angle was 167 deg., as shown in figure 2.
Example 3
(1) Sequentially adding absolute ethyl alcohol, deionized water, ammonia water and tetraethoxysilane into a reaction bottle according to a molar ratio of 40:10:0.18:1, reacting for 2 hours at a constant temperature of 25 ℃, and then aging for 7 days at a constant temperature of 25 ℃ in a sealing manner to obtain SiO 2 And (3) sol.
(2) To SiO 2 Adding hexamethyldisilazane into the sol according to the mol ratio of 1.11:1 of hexamethyldisilazane to tetraethoxysilane, reacting for 2 hours at the constant temperature of 25 ℃, and aging for 7 days at the constant temperature of 30 ℃ in a sealing way to obtain the hydrophobic modified SiO 2 And (3) sol.
(3) Immersing a glass substrate into hydrophobically modified SiO 2 Coating film in sol at 6000 μm/s and drying at room temperature.
The refractive index of the obtained antireflection film is 1.25, and the transmittance thereof at 754nm is 99.85%, as shown in FIG. 1; the water contact angle was 163 °, as shown in fig. 2.
FIG. 1 shows that control 2 increases the water content of the sol formulation compared to control 1, resulting in an increase in the refractive index of the film, resulting in a decrease in transmittance; comparative example 3 SiO was treated with hexamethyldisilazane under the same water content and other conditions as comparative example 1 2 The sol is hydrophobically modified, and the refractive index of the obtained film is reduced, which also results in reduced transmittance.
FIG. 2 shows that control 2 increases the water content of the sol formulation and decreases the film contact angle as compared to control 1; comparative example 3 use of hexamethyldisilazane to SiO 2 The sol is subjected to hydrophobic modification, so that the contact angle of the film is increased, and the super-hydrophobic effect is achieved.
Thus, comparative examples 1 to 3 show that SiO can be improved by increasing the water content 2 Refractive index of film by using hexamethyldisilazane to SiO 2 Hydrophobic modification of the sol can reduce SiO 2 Refractive index of the film.
Examples 1 to 3 are control SiO 2 Water content in sol and use of hexamethyldisilazane to SiO 2 The sol is hydrophobically modified. FIG. 1 shows that examples 1-3 produce antireflection films with peak permeabilities greater than 99.8%; FIG. 2 shows that the films produced in examples 1-3 have contact angles greater than 160.
Thus, examples 1-3 demonstrate that by controlling SiO 2 Water content in sol and use of hexamethyldisilazane to SiO 2 The sol is subjected to hydrophobic modification to obtain the super-high transmittance>99.8%) and superhydrophobicity>160 deg. antireflection film.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. The preparation method of the high-transmittance superhydrophobic antireflection film is characterized by comprising the following steps of:
(1) Sequentially adding absolute ethyl alcohol, deionized water, ammonia water and tetraethoxysilane into a reaction bottle, reacting at constant temperature, sealing and aging to obtain SiO 2 Sol;
(2) To the SiO produced in step (1) 2 Adding hexamethyldisilazane into the sol, reacting at constant temperature, sealing and aging to obtain hydrophobically modified SiO 2 Sol;
(3) Adopting a dipping-pulling method to prepare the hydrophobically modified SiO in the step (2) 2 Plating the sol on the surface of a glass substrate, airing at room temperature, and finally obtaining the high-transmittance superhydrophobic antireflection film;
the molar ratio of the absolute ethyl alcohol to the deionized water to the ammonia water to the tetraethoxysilane in the step (1) is (30-40): 6-12): 0.15-0.18): 1;
the molar ratio of hexamethyldisilazane in step (2) to ethyl orthosilicate in step (1) (0.37-1.11): 1.
2. The method of manufacturing according to claim 1, characterized in that: the temperature of the constant temperature reaction in the step (1) is 25-30 ℃ and the time is 1-6h; the temperature of the sealing and aging is 25-30 ℃ and the time is 7-10 days.
3. The method of manufacturing according to claim 1, characterized in that: the temperature of the constant temperature reaction in the step (2) is 25-30 ℃ and the time is 1-6h; the temperature of the sealing and aging is 25-30 ℃ and the time is 5-10 days.
4. The method of manufacturing according to claim 1, characterized in that: the speed of pulling the glass substrate out of the sol in the step (3) is 1000-6000 mu m/s.
5. The high-transmittance superhydrophobic antireflection film prepared by the preparation method according to any one of claims 1 to 4.
6. The high-transmittance superhydrophobic antireflection film of claim 5, wherein: the thickness of the high-transmittance super-hydrophobic antireflection film is 81-183nm, and the refractive index is 1.21-1.25.
7. The high-transmittance superhydrophobic antireflection film of claim 5, wherein: the peak transmittance of the high-transmittance super-hydrophobic antireflection film is greater than 99.8%, and the water contact angle is greater than 160 °.
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