CN112110654A - Preparation method and application of optical anti-reflection antifogging film - Google Patents
Preparation method and application of optical anti-reflection antifogging film Download PDFInfo
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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
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
- C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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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
- C03C2217/73—Anti-reflective coatings with specific characteristics
- C03C2217/732—Anti-reflective coatings with specific characteristics made of a single layer
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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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- 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
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/31—Pre-treatment
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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
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to the field of optical materials, and particularly relates to a preparation method and application of an optical anti-reflection antifogging film. The preparation method comprises the following steps: dissolving allyl triethoxysilane and ethyl orthosilicate in absolute ethyl alcohol, adding distilled water, and adding hydrochloric acid while stirring to obtain the organic silicon polymer sol. The optical substrate is treated by a mixture of concentrated sulfuric acid and hydrogen peroxide and then ultrasonically cleaned. Soaking the cleaned substrate in organosilicon polymer sol by a dipping-pulling method, taking out the substrate after standing, and N2And drying in the atmosphere to obtain the organic silicon optical film. And soaking the prepared film in an ozone water solution to prepare the optical anti-reflection antifogging film. With enhanced film formation by ozone treatmentHydrophilic, when the fog drops contact the surface of the film, the fog drops can spread to form a uniform water film, so that light refraction and reflection caused by the fog drops are avoided, and the light transmittance of the substrate is improved. Meanwhile, the protruding structure on the surface of the film is etched by soaking, and the roughness of the surface of the film is reduced.
Description
Technical Field
The invention belongs to the field of optical materials, and particularly relates to a preparation method and application of an optical anti-reflection antifogging film.
Background
Transparent materials have important roles in people's lives, such as glass of windows, glasses and lenses, automobile windshields, mobile phone screens and the like, which are not separated from the application of the transparent materials. When the ambient temperature changes greatly or the humidity is high, water vapor can be condensed into fog drops on the surface of the material, so that the light transmittance of the material is reduced, inconvenience is brought to production and life, and even accidents are caused. A common method for improving the antifogging property of a material is to coat a smooth hydrophilic film on the surface of the material, wherein the smooth hydrophilic film can enable water vapor to form a uniform water film on the surface of the material, so that the light transmittance is improved. However, conventional antifogging coatings have low stability and cannot be used for a long time. Therefore, the development of the anti-reflection antifogging film with good stability is of great significance.
Disclosure of Invention
Aiming at the problems, the invention utilizes ozone to oxidize carbon-carbon double bonds of carbon chains at the side ends of an organic silicon network into carboxyl, carries out surface modification on a transparent substrate, and develops an antifogging material which can be firmly connected with transparent substrates such as optical glass and the like and has high hydrophilicity and high light transmittance.
The specific scheme is as follows:
(1) dissolving precursors of Allyl Triethoxysilane (ATES) and Tetraethoxysilane (TEOS) in absolute ethyl alcohol, adding a certain amount of distilled water, and adding a certain amount of hydrochloric acid for reaction while stirring to obtain the organic silicon polymeric sol.
Wherein, the structural formula of the organosilicon precursor allyl triethoxysilane is as follows:
ATES, TEOS, absolute ethanol, H2O: the HCl molar ratio is 1:1: 2-5: 20-60:0.5～0.8。
the stirring temperature is 50-80 ℃, and the reaction time is 2-5 h.
(2) Putting a transparent optical substrate into a beaker, adding a proper amount of concentrated sulfuric acid and hydrogen peroxide into the beaker, heating until no bubbles are generated in the beaker, respectively ultrasonically cleaning the substrate with distilled water and absolute ethyl alcohol after the substrate is cooled to room temperature, and performing ultrasonic cleaning on the substrate in N2Drying in the atmosphere for coating.
Wherein the volume ratio of concentrated sulfuric acid to hydrogen peroxide is 0.4-1.0: 1.
heating at 50-75 deg.C, and ultrasonic treating for 5-15 min.
(3) Soaking the substrate treated in the step (2) into organic silicon polymer sol by using a dipping-pulling method, standing for a period of time, taking out the substrate, putting the substrate into an oven, and putting the substrate into N2Drying in the atmosphere, and stopping introducing N2And raising the temperature to 100 ℃ by a program, and naturally cooling to room temperature to obtain the optical film.
The specific process is as follows: firstly, a substrate is immersed into organic silicon polymer sol, then the substrate is lifted upwards, suspended and kept stand for 5min, then the substrate is turned around, and the steps are repeated, suspended, so as to ensure that the film thickness is uniform.
Wherein, the specific operation of the temperature programming is as follows: keeping the temperature at 25 deg.C for 5-10min, keeping the temperature at 5 deg.C for 5-10min, keeping the temperature at 100 deg.C for 15-25min, and naturally cooling to room temperature to obtain the final product.
(4) And (4) soaking the optical film prepared in the step (3) in an ozone water solution to obtain the modified optical anti-reflection antifogging film.
Wherein the concentration of the ozone water solution is 0.5-5ppm, the soaking time is 5-10min, and the soaking temperature is normal temperature.
The ozone treatment is to oxidize double bonds on the allyl triethoxysilane into carboxyl groups, thereby improving the hydrophilicity of the film, spreading liquid drops on the surface of the film, forming a more uniform water film, thereby avoiding the refraction and reflection of light generated by the water drops and ensuring the light transmittance of the glass substrate.
The optical anti-reflection antifogging film prepared by the method.
(1) According to the invention, allyl triethoxysilane and tetraethoxysilane are copolymerized to generate a-Si-O-Si-network, the-Si-O-Si-network can form firm connection with the surface of the transparent optical glass, firm adhesion of a film layer is ensured, the film layer is not easy to fall off, and meanwhile, two types of organic silicon are copolymerized to form a covalent bond structure, so that the stability of the film is higher than that of a common film.
(2) The optical film is subjected to ozone treatment, carbon-carbon double bonds (-C ═ C-) at the side end are oxidized into carboxyl (-COOH), the hydrophilicity of the film is enhanced, and when fog drops contact the surface of the film, the fog drops can spread to form an even water film, so that light refraction and reflection caused by the fog drops are avoided, and the light transmittance of the substrate is improved. Meanwhile, some protruding structures on the surface of the film are etched away by soaking in the ozone water solution, the surface of the film gradually becomes smooth, and the roughness is reduced. In the case of a hydrophilic film, the roughness is reduced, the surface of the film becomes smooth, the contact angle with water is reduced, and the hydrophilicity is improved, thereby enhancing the antifogging property and the light transmittance.
(3) The invention adopts low-concentration ozone water solution for surface post-treatment, the structure of the transparent substrate can not be damaged, the light transmittance of the prepared hydrophilic antireflection film is less influenced by air humidity, and liquid drops can be spread on the surface of the film under the condition of different air humidity to form a more uniform water film.
Drawings
FIG. 1 is a chemical reaction mechanism diagram of the anti-reflection antifogging film.
Fig. 2 is an AFM image of the thin films prepared in example 1 and comparative example 1.
Fig. 3 is an AFM image of the thin films prepared in comparative example 2 and comparative example 3.
FIG. 4 is an AFM image of a thin film prepared in comparative example 4.
Detailed Description
Example 1
(1) Preparing precursor sol: dissolving precursors of Allyl Triethoxysilane (ATES) and Tetraethoxysilane (TEOS) in absolute ethyl alcohol, adding distilled water, and adding hydrochloric acid while stirring for reaction to obtain the organic silicon polymer sol. Wherein, ATES, TEOS, absolute ethyl alcohol and H2O, HCl in a molar ratio of 1:1:2:60:0.8. The stirring temperature is 60 ℃, and the reaction time is 3 h.
(2) Optical substrate pretreatment: putting a transparent optical substrate into a beaker, adding concentrated sulfuric acid and hydrogen peroxide which can immerse the optical substrate into the beaker, heating until no bubbles are generated in the beaker, respectively ultrasonically cleaning the substrate for 5min by using distilled water and absolute ethyl alcohol after the substrate is cooled to room temperature, and performing ultrasonic cleaning on the substrate in N2Drying in the atmosphere for coating. Wherein the volume ratio of concentrated sulfuric acid to hydrogen peroxide is 1:1, the heating temperature is 65 ℃, and the ultrasonic time is 5 min.
(3) Coating and curing: immersing the substrate treated in the step (2) into the organic silicon polymer sol prepared in the step (1), then lifting upwards, suspending and standing for 5min, turning the substrate around, repeating the steps, suspending and standing for 5min to ensure uniform film thickness, taking out the substrate, putting the substrate into an oven, and putting the substrate in an N (nitrogen) atmosphere2Drying in the atmosphere, and stopping introducing N2And raising the temperature to 100 ℃ by a program, and naturally cooling to room temperature to obtain the optical film. Wherein, the specific operation of the temperature programming is as follows: keeping the temperature at 25 deg.C for 10min, and keeping the temperature at 5 deg.C for 5 min. When the temperature is raised to 100 ℃, keeping the temperature for 20min, and then naturally cooling to the room temperature to obtain the optical film.
(4) Ozone treatment: and (4) soaking the optical film prepared in the step (3) in an ozone water solution to obtain the modified optical anti-reflection antifogging film. Wherein the concentration of the ozone water solution is 1ppm, the soaking time is 5min, and the soaking temperature is normal temperature.
Comparative example 1
Compared with example 1, the difference is that: and preparing the optical film without ozone treatment.
The preparation method of step (1) to step (3) is the same as that of example 1.
Fig. 2 is an AFM image of the thin films prepared in example 1 and comparative example 1. The left figure is the AFM picture of the film after ozone treatment, part of the protruding structure on the film surface is etched away after ozone treatment, and the surface roughness is reduced, and the right figure is the AFM picture of the film without ozone treatment.
Comparative example 2
Comparative example 1 is different from example 1 in that: the temperature in step (3) was raised to 60 ℃ (curing temperature), and the preparation method was the same as example 1.
Comparative example 3
Comparative example 2 is different from example 1 in that: the temperature in step (3) was raised to 150 ℃ (curing temperature), and the preparation method was the same as example 1.
Fig. 3 is an AFM image of the thin films prepared by implementing comparative example 2 and comparative example 3. The left graph shows the AFM of the thin film at a curing temperature of 60 ℃ and the right graph shows the AFM of the thin film at a curing temperature of 150 ℃. It can be seen from the figure that the surface of the film was relatively rough although the film was subjected to ozone treatment at a curing temperature of 60 ℃ or 150 ℃.
Comparative example 4
Compared with example 1, the difference is that: the organosilicon precursor used was different, propyltriethoxysilane was used as precursor, the preparation method was the same as in example 1, and the ozone treatment was performed.
FIG. 4 is an AFM image of a thin film prepared in comparative example 4. Propyl triethoxysilane was used as the organosilicon precursor to prepare the optical film. After ozone treatment, the average roughness of the surface of the film is reduced.
The optical substrates prepared in each of examples and comparative examples were subjected to water contact angle and light transmittance tests (light transmittance of the film was measured using an ultraviolet spectrophotometer) as detailed in table 1.
TABLE 1
| Sample (I) | Water contact angle theta | Light transmittance (%) | Average roughness (nm) |
| Example 1 | 27.1° | 95.6 | 63.75 |
| Comparative example 1 | 54.3° | 90.7 | 85.12 |
| Comparative example 2 | 42.3° | 92.4 | 74.25 |
| Comparative example 3 | 44.2° | 92.1 | 78.32 |
| Comparative example 4 | 55.1° | 91.3 | 68.43 |
Claims (10)
1. The preparation method of the optical anti-reflection antifogging film is characterized by comprising the following steps:
(1) dissolving precursors of Allyl Triethoxysilane (ATES) and Tetraethoxysilane (TEOS) in absolute ethyl alcohol, adding distilled water, and adding hydrochloric acid while stirring for reaction to prepare organic silicon polymer sol;
(2) putting a transparent optical substrate into a beaker, adding concentrated sulfuric acid and hydrogen peroxide into the beaker, heating until no bubbles are generated in the beaker, and respectively distilling the substrate after the substrate is cooled to room temperatureUltrasonic cleaning with water and absolute ethyl alcohol under N2Drying in the atmosphere for coating;
(3) soaking the substrate treated in the step (2) into organic silicon polymer sol by using a dipping-pulling method, standing, taking out the substrate, putting the substrate into an oven, and putting the substrate into N2Drying in the atmosphere, and stopping introducing N2Heating to 100 deg.c and cooling naturally to room temperature to obtain optical film;
(4) and (4) soaking the optical film prepared in the step (3) in an ozone water solution to obtain a modified optical antifogging film.
2. The preparation method of the optical anti-reflection antifogging film according to claim 1, characterized in that: the structural formula of the precursor is as follows:
3. the preparation method of the optical anti-reflection antifogging film according to claim 1, characterized in that: ATES, TEOS, absolute ethyl alcohol and H in step (1)2O: the HCl molar ratio is 1:1: 2-5: 20-60: 0.5 to 0.8.
4. The preparation method of the optical anti-reflection antifogging film according to claim 1, characterized in that: in the step (1), the stirring temperature is 50-80 ℃, and the reaction time is 2-5 h.
5. The preparation method of the optical anti-reflection antifogging film according to claim 1, characterized in that: the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide in the step (2) is 0.4-1.0: 1.
6. The preparation method of the optical anti-reflection antifogging film according to claim 1, characterized in that: in the step (2), the heating temperature is 50-75 ℃, and the ultrasonic time is 5-15 min.
7. The preparation method of the optical anti-reflection antifogging film according to claim 1, characterized in that: in the step (3), the substrate is firstly immersed into the organic silicon polymer sol, then is lifted upwards, is suspended and stands, then is turned around, and is repeated, and is suspended and dried to ensure that the film thickness is uniform.
8. The preparation method of the optical anti-reflection antifogging film according to claim 1, characterized in that: the specific operation of the temperature rise in the step (3) is as follows: keeping the temperature at 25 deg.C for 5-10min, keeping the temperature at 5 deg.C for 5-10min, keeping the temperature at 100 deg.C for 15-25min, and naturally cooling to room temperature to obtain the final product.
9. The preparation method of the optical anti-reflection antifogging film according to claim 1, characterized in that: in the step (4), the concentration of the ozone water solution is 0.5-5ppm, the soaking time is 5-10min, and the soaking temperature is normal temperature.
10. An optically anti-reflective anti-fog film prepared according to the method of any one of claims 1 to 9.
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