JP3579655B2 - Transparent substrate having antifouling hydrophobic coating and method for producing the same - Google Patents

Description

[0001]
(Background of the Invention)
The present invention relates to optical thin film coatings and methods of applying such coatings, and more particularly, to methods of applying hydrophobic, stain-resistant optical thin film coatings.
Many optical transparencies (transparencies, such as transparencies) include coatings made by laminating multiple thin film layers with precise thickness and refractive index. Usually, when such coatings are obtained from inorganic materials, their exposed surfaces are inherently hydrophobic and have a high surface energy. As a result, foreign contaminants in the form of dust, oil and fingerprints adhere strongly to such exposed surfaces.
[0003]
Such extraneous contaminants can significantly reduce the optical performance of such coatings by partially altering the path of the incident light. Also, the attachment of such foreign contaminants can be very strong, so that they can only be removed by applying various chemical cleaning agents or by physical removal. However, such cleaning methods can permanently damage the coating and / or the underlying substrate.
[0004]
One prior art technique for reducing the surface energy of such inorganic coatings is by heat treating the coated substrate at a temperature in the range of 400-800 ° C and dehydroxylating the -OH groups on its surface. is there. This technique is usually insufficient to treat surfaces already exposed to the surrounding environment and cannot be used to treat coatings applied to substrates made of plastic. This is because plastic substrates typically have a deformation temperature that is lower than the processing temperature.
[0005]
Another prior art technique for reducing the surface energy of such inorganic coatings involves modifying the surface using chemical vapor deposition. Unfortunately, this technique requires the use of relatively expensive vacuum equipment, and requires relatively long reaction times and time to evacuate chemicals from the chamber.
[0006]
Yet another prior art technique for reducing the surface energy of such inorganic coatings is to deposit a hydrophobic overcoat containing saturated hydrocarbons, fluorocarbons or organosilanes over the optical coating. That is. Organosilane-based solutions usually contain non-polar or less polar solvents such as octane, heptane, toluene, tetrahydrofuran, trichloroethane, etc., which are highly flammable or toxic. Therefore, it is not desirable to use these solvents. Known techniques for grafting an organic silane coating to an underlying coated substrate are also known to soak under a dry atmosphere (dry nitrogen or dry air) for a relatively long period of time, soaking with a solvent. It is necessary to wash or wipe and then heat dry at high temperature. If the coating is applied in a higher humidity environment, the coating solution will degrade and / or the coating will be uneven or translucent.
[0007]
In addition, organosilane coatings typically have optical coefficients very similar to the optical coefficients of glass, such that when such coatings are applied to glass substrates, they may not be readily visible. I don't know. However, any slight variation in coating thickness can adversely affect the optical performance of many optical substrates with multilayer thin film coatings, making surface contaminants and defects prominent.
[0008]
Thus, a low cost, effective optical thin film coating that is hydrophobic, oil-repellent and antifouling without adversely affecting the desired optical properties of any underlying coating and / or transparent substrate. It should be appreciated that there is a need for a method for applying the above-described stain-resistant coating to its transparent substrate. The hydrophobic coating is also chemically stable (ie, does not react with various solvents and cleaning agents) and is also mechanically and environmentally stable (ie, changes in temperature, humidity and UV light). Endure). In addition, the hydrophobic coating is uniform, free of pinholes or spot defects, and its application should not be limited to any particular substrate size. Furthermore, the hydrophobic coating should be applied by a simple dip-coating procedure that does not use toxic or highly flammable solvents, and the hydrophobic coating is environmentally friendly It should not require the need for wiping or cleaning during the application process (no harm to the environment). The present invention fulfills these needs and provides further related advantages.
[0009]
(Summary of the Invention)
The present invention relates to an optical thin film coating which is hydrophobic, oil repellent and stain resistant which does not adversely affect the desired optical properties of any underlying coating and / or transparent substrate. And a method for applying the coating. The hydrophobic coating is chemically stable (i.e., does not react with various solvents and cleaning agents), but is also mechanically and environmentally stable (i.e., changes in temperature, humidity, and ultraviolet light). Endure). In addition, the hydrophobic coating is uniform, has no pinholes or spot defects, and its application is not limited to any particular substrate size. Further, the hydrophobic coating is applied without the use of toxic or highly flammable solvents, yet the hydrophobic coating is environmentally friendly and requires the need for wiping and cleaning during the application process. do not do.
[0010]
More specifically, this hydrophobic, oil-repellent, antifouling thin film coating comprises an organosilane in a solvent containing water; alcohols such as ethanol, propanol, butanol; ethylene glycol or glycerol; and an acid catalyst. It is prepared by immersing the substrate in the contained processing solution. The organosilane is preferably in a concentration ranging from 0.05 to 50 mmol per 1000 ml of solution, the solvent comprising 0.1 to 90% by weight of water and 0.5 to 20% by weight of ethylene glycol and / or glycerol. The remaining amount is alcohol (preferably ethanol or propanol alone or mixed with butanol). The treatment solution is preferably prepared in a two-step procedure. In a two-step procedure, the organosilane is reacted first in concentrated form and then diluted and reacted.
[0011]
The organosilane contained in the processing solution has a saturated or fluorinated hydrocarbon chain. This hydrocarbon chain is directly linked to the silicon atoms in the underlying substrate by C-Si bonds. The organosilane further has 1 to 3 hydrolyzable groups. These groups are directly bonded to a silicon atom by a bond of C—O—Si. This organosilane has the formula:
_{(RO) 3-n -Si -} {[C p + q H 2p F 2q] - (CH 3 or _{-CF 3)} 1 + n}
Wherein n is 0-3, p + q ≧ 2 (preferably> 8), and R is an alkyl group (preferably CH ₃ — or CH ₃ CH ₂ —). it can.
[0012]
The acid catalyst contained in the treatment solution is an inorganic or organic acid, preferably CH ₃ CO ₂ H, HCl or HNO ₃ .
The dip coating procedure requires that the substrate be immersed in the processing solution for only 1 to 60 seconds and then pulled up at a rate of about 0.001 cm / sec or more. It can be applied to substrates of any size, and can be immersed simultaneously, with the constraint that multiple substrates are spaced at least 1 cm apart. The relative humidity during the dip coating procedure should be in the range 15-95%, preferably 40-80%. The temperature should be in the range 10-40 ° C. The dip-coated substrate is flash dried at room temperature for at least 1 minute (preferably 20 minutes) and then heat dried at a temperature in the range of 50-250 ° C for at least 1 minute.
[0013]
The surface of the substrate coated according to the present invention may be, for example, a metal component such as SiO ₂ , Al ₂ O ₃ , ZnO ₂ , TiO ₂ , ITO, In ₂ O ₃ , Sb ₂ O ₃ , MgF ₂ , SnO ₂ or Should contain inorganic components. These surfaces can be formed by bulk materials, by coating of such components on an underlying substrate, or by organic / inorganic composites containing such inorganic components.
Other features and advantages of the invention will be apparent from the following description of preferred embodiments and methods. These are described with reference to the accompanying drawings, which illustrate, by way of example, the principles of the invention.
[0014]
(Description of preferred method)
A preferred embodiment of the present invention is a specific hydrophobic protective coating (overcoat) which is an inorganic, non-reflective multilayer coating on which the coated substrate has a substantially reduced soil susceptibility to staining. , Overcoat) in the form of a transparent plastic substrate having the multilayer coating deposited thereon. In addition, the overcoat is applied in an effective manner without the need for highly flammable or toxic solutions and without the need for long processing times. In particular, the hydrophobic protective film is obtained by dip-coating the substrate in an aqueous-alcoholic solution containing a fluorinated organosilane, and then drying the coated substrate at a predetermined temperature for a predetermined time and then heating and drying. To apply.
[0015]
The solvent used for the fluorinated organosilane solution contains water and an alcohol such as ethanol, propanol, or butanol. The solvent optionally further contains an organic solvent having a boiling point higher than that of the alcohol, such as ethylene glycol and glycerol. All of these solvent components are less flammable and are less toxic than the solvents used in prior art methods for applying similar hydrophobic coatings.
[0016]
The organosilane used in the preferred embodiment of the present invention contains a saturated hydrocarbon chain bonded directly to the metal atom by a CO-metal bond. The carbon chain may be branched, but contains at least 2, preferably 8 or more carbon atoms. A hydrogen atom bonded to a carbon atom may be replaced by a fluorine atom such as a pre-fluorinated carbon chain or a fluorinated carbon chain. The organosilane preferably has 1 to 3 hydrolyzable groups that are directly bonded to the metal atom by a CO-metal bond. This organosilane has the formula:
_{(RO) 3-n -Si -} {[C p + q H 2p F 2q] - (CH 3 or _{-CF 3)} 1 + n}
Wherein n is 0-3, p + q ≧ 2 (preferably> 8), and R is an alkyl group (preferably CH ₃ — or CH ₃ CH ₂ —). it can.
[0017]
The processing solution _{also, CH 3 CO 2 H, HCl} , may contain a suitable acid catalyst such as HNO _3.
The concentration of the organosilane in the treatment solution is in the range of 0.05 to 50 mmol per 1000 ml of the solution, preferably in the range of 0.1 to 10 mmol per 1000 ml of the solution. The solvent contains 0.1-90% by weight of water and 0.5-20% by weight of ethylene glycol and / or glycerol. The remainder of the solvent is alcohol (preferably ethanol or propanol alone or mixed with butanol).
[0018]
The composition of the processing solution and the method of preparing the processing solution have a significant effect on the properties of the resulting coating. For example, depending on the details of the method of preparing the processing solution and depending on the method of applying the processing solution, processing solutions containing the same organosilane (or even the same processing solution) have been improved; or Unaltered; or severely or permanently contaminated (e.g., containing translucent or non-removable stains); non-staining (anti-contaminant) and hydrophobic It can be used to make a dipped substrate.
[0019]
The non-staining and hydrophobic coating of the present invention may be, for example, a metal component such as SiO ₂ , Al ₂ O ₃ , ZnO ₂ , TiO ₂ , ITO, In ₂ O ₃ , Sb ₂ O ₃ , MgF ₂ , SnO _2. Alternatively, it is suitable for applying to a substrate containing an inorganic component. The substrate can be made of a bulk material such as a glass sheet, aluminum foil, or the like. Alternatively, the substrate itself can be a coating of an inorganic component formed on any suitable substrate. The substrates are preferably, but not necessarily, cleaned and free of surface contamination prior to application of the non-staining, hydrophobic coating. Other features of the present invention will be apparent from the following description of non-limiting examples.
[0020]
Example 1
Processing solutions were prepared in a two-step procedure. First, solution A was mixed with isopropanol, water, HCl and 1H, 1H, 2H, 2H-perfluorodecyltriethoxysilane in a relative molar ratio of 1300: 11: 290: 1 and magnetically stirred for 2 hours. Prepared. Next, solution A was mixed with solution B containing 56000 parts (molar ratio) of water, 1500 parts of ethylene glycol, and 15000 parts of isopropanol, and magnetically stirred for 1 hour to produce a treatment solution.
[0021]
A substrate (40 cm x 15 cm) of polymethyl methacrylate (PMMA) with a multilayer non-reflective (AR) inorganic coating is then contacted with the treatment solution for 10 seconds, and then exposed to 0,5% relative humidity at 50%. It was withdrawn from the processing solution at a speed of 15 cm / sec. The substrate was then evaporated in open air for 20 minutes and then heat dried at 84 ° C. for an additional 20 minutes. The measured contact angle of water with the coated substrate was 55 ° before treatment and 118 ° after treatment. The greater the contact angle, the greater the degree of hydrophobicity. No visible defects were observed in the treated substrate, and no shift in the optical performance of the treated substrate in the spectral region of 400-700 nm was observed.
The improved soil resistance of the treated substrate made in Example 1 is shown in FIG. Also, no degradation in the optical performance of the treated substrate is seen, as indicated by the reflectivity over the 400-700 nm spectral region of FIG.
[0022]
Example 2
The treatment solution was prepared in exactly the same way as performed in Example 1, except that the reaction time for preparing Solution A was reduced to 30 minutes. An AR-coated PMMA substrate was contacted with the treatment solution for 10 seconds and then pulled up at a rate of 0.15 cm / sec at 50% relative humidity. The substrate was then heat dried at 84 ° C. for 20 minutes. As a result of measuring the contact angle of water, it was increased from 55 ° before the treatment to only 70 ° after the treatment. No visible defects were observed on the treated substrate. This example shows that the reaction time for preparing solution A was insufficient.
[0023]
Example 3
First, solution A was mixed with isopropanol, water, HCl and 1H, 1H, 2H, 2H-perfluorodecyltriethoxysilane in a relative molar ratio of 1000: 3: 1: 1 and magnetically stirred for 30 minutes. A preparation solution was prepared by the preparation. Solution A was then mixed with an additional 5500 parts (molar ratio) of isopropanol and magnetically stirred for 15 hours. An AR-coated PMMA substrate was contacted with the treatment solution for 20 minutes and then pulled up at a rate of 0.3 cm / sec at 50% relative humidity. The substrates were then heat dried at 84 ° C. for 20 minutes. As a result of measuring the contact angle of water, the contact angle increased from 55 ° before the treatment to 116 ° after the treatment.
[0024]
Many visible defects were not observed on the treated substrate. This may be due to the presence of a non-uniform, agglomerated layer of organosilane on the substrate. The particular solvent used, rather than the particular organosilane, appears to be an important parameter. Defects and stains on the treated substrate can be partially removed by washing with isopropanol and then wiping with a cotton cloth. However, if this washing is performed before heat drying, the organosilane molecules are prevented from binding to the substrate and the water contact angle remains constant at 55 ° after treatment.
[0025]
Example 4
First, isopropanol, water, HCl and 1H, 1H, 2H, 2H-perfluorodecyltriethoxysilane were mixed at a molar ratio of 1800: 74: 2.3: 1, and the solution A was mixed by magnetic stirring for 6 hours. Was prepared to prepare a treatment solution. Solution A was then mixed with an additional 23,000 parts of water (molar ratio) and magnetically stirred for 30 minutes.
[0026]
An AR-coated PMMA substrate was contacted with the treatment solution for 10 seconds and then pulled up at a rate of 0.2 cm / sec at 50% relative humidity. The substrates were then heat dried at 84 ° C. for 20 minutes without preliminary flash drying in open air. As a result of measuring the contact angle of water, the contact angle increased from 55 ° before the treatment to 112 ° after the treatment. No visible defects were observed on the treated substrate. However, the useful life of the treatment solution was measured to be only about 30 hours. Substrates treated with the treatment solution three days after preparing the treatment solution did not show any significant increase in water contact angle. This indicates that the particular solvent used is important in determining the useful life of the processing solution.
[0027]
Example 5
A processing solution was prepared in exactly the same manner as performed in Example 1. The AR-coated PMMA substrate was dip coated in the processing solution in exactly the same manner as performed in Example 1. The first set of dip-coated substrates was flashed in open air for 20 minutes and then baked at 40 ° C. for 10 minutes. As a result of measuring the water contact angle of the first set of substrates, the water contact angle increased from 55 ° before the treatment to 86 ° after the treatment. The second set of dip coated substrates was immediately heat dried at 84 ° C. for 20 minutes without pre-evaporation in open air. As a result of measuring the water contact angle of the second set of substrates, the angle increased from 55 ° before the treatment to 95 ° to 120 ° after the treatment. Many visible spot defects and organosilane fouling adhered strongly to both sets of treated substrates. This example shows that the curing conditions are insufficient, that is, the temperature of the heating and drying is not high enough, or evaporation in open air has been omitted.
[0028]
Example 6
A processing solution and an AR-coated PMMA substrate were prepared in exactly the same manner as in Example 1, except that the relative humidity during withdrawal of the substrate from the processing solution was reduced to 10%. As a result of measuring the water contact angle of these treated substrates, the angle increased from 55 ° before the treatment to 95 to 120 ° after the treatment. Many visible spot defects and organosilane stains adhered strongly to these substrates. This example shows that the relative humidity during withdrawal of the substrate from the processing solution affects the properties of the resulting coating.
[0029]
Example 7
Example 1 was repeated, except that 1H, 1H, 2H, 2H-perfluorodecyltrichlorosilane, octadecyltrichlorosilane and octadecyltriethoxysilane were used instead of 1H, 1H, 2H, 2H-perfluorodecyltriethoxysilane. Three treatment solutions were prepared in exactly the same way. The AR-coated PMMA substrate was then dip coated in exactly the same way as performed in Example 1. As a result of measuring the water contact angle of these treated substrates, the angle increased from 55 ° before the treatment to 100 ° to 120 ° after the treatment. This example shows that the present invention has the utility of using various organosilane compositions.
[0030]
Example 8
The treatment solution and the AR-coated PMMA substrate were prepared in exactly the same manner as in Example 1, except that the treatment solution was aged at room temperature for 60 days. It was confirmed that the substrates treated with the cured solution had substantially the same properties as the substrates treated with the solution just obtained. This example shows that curing of the preferred treatment solution does not adversely affect the usefulness of the treatment solution.
[0031]
Example 9
For AR-coated PMMA substrates treated in the manner disclosed in Example 1, (1) thermal shock test (-30-80 ° C., 1000 cycles), (2) dry cotton abrasion test (500 g weight, 1000 times) (3) UV test (carbon arc, 450 hours), (4) Humidity test (60 ° C, 95% relative humidity, 192 hours), and (5) Chemical resistance test (gasoline, detergent, 60 ° C, 24 hours). It was confirmed that there was no significant change in the antifouling properties and hydrophobicity of the substrates tested.
[0032]
Example 10
A pair of AR-coated eyeglasses were dip-coated in a treatment solution similar to the treatment solution prepared in Example 1 and then dried overnight (15 hours) at room temperature. The treated glasses were found to have greater resistance to fingerprints and dust contamination. The frequency of the need to clean treated glasses has been reduced by 400-1000%. In addition, it has been found that the treated eyeglasses are much easier to clean than untreated eyeglasses.
[0033]
Example 11
An AR-coated PMMA substrate (40 cm x 35 cm) was dip coated in a processing solution prepared in the same manner as described in Example 1. It was confirmed that about 95% of the substrate surface had an initial water contact angle of 65 ° and the remaining about 5% of the substrate surface had an initial water contact angle of 77 °. This latter contamination of the surface is believed to be due to such fluctuations in the water contact angle. After dip coating and heat drying the coated substrate in the same manner as described in Example 1, the water contact angle increases to 115-120 ° for the region where the initial water contact angle was 65 °. However, it was confirmed that the region where the initial water contact angle was 77 ° did not substantially change.
[0034]
A new treatment solution was prepared in the same manner as performed in Example 1, except that the amount of solution A was increased relative to the amount of solution B. In short, the same amount of solution A as in Example 1 was added to a fresh solution B containing 44800 parts of water (molar ratio), 1200 parts of ethylene glycol and 12000 parts of isopropanol. After treating the substrate according to the same procedure as described in Example 1, a uniform, antifouling hydrophobic coating was applied to the entire surface of the substrate, and then the water contact angle was measured, resulting in 115-120 across the surface. °. This example shows that by increasing the concentration of the organosilane in the processing solution, the adverse effects associated with fouling of the underlying AR coating can be overcome.
[0035]
Example 12
After extensive use and / or prolonged curing of the treatment solution prepared as described in Example 1, the treatment solution produced a coating with an appreciable increase in water contact angle. After adding more than 30% of the solution A to the old processing solution and pre-reacting for 2 hours, stirring the replenished solution for 10 minutes or more, such old processing solution can be used for the initial effective solution. Sex can be regained. Such a replenishment solution produced a uniform, antifouling hydrophobic coating over the surface of the AR-coated PMMA substrate. This example shows that the processing solution can be replenished without discarding old solvent and without producing any waste solution.
While the invention has been described in detail only in terms of the presently preferred embodiments and methods, those skilled in the art will recognize that various modifications may be made without departing from the invention.
[Brief description of the drawings]
FIG. 1 shows the effect of applying a permanent marker to a transparent substrate having an inorganic non-reflective multilayer coating. Here, the left side of the figure is untreated, and the right side is treated with a hydrophobic protective film according to the present invention.
FIG. 2 is a graph showing the reflectance of a transparent substrate having an inorganic non-reflective multilayer coating and having and not having a hydrophobic protective film according to the present invention.

Claims (27)

A method of applying an antifouling, hydrophobic optical coating to a transparent substrate,
Essentially, organosilane, an alcohol, a first solution having containing water and an acid catalyst to prepare,
The organosilane mixed in the first solution is
Next formula
_{(RO) 3-n -Si- {} [C p + q H 2p F 2q] - (CH 3 Or -CF ₃ ) ｝ _{1 + n}
Wherein n is 0 to 3, p + q ≧ 2, and R is an alkyl group.
1H, 1H, 2H, 2H-perfluorodecyltrichlorosilane,
Octadecyltrichlorosilane, and
Selected from the group consisting of mixtures thereof,
The first solution was reaction,
Mixing a second solution containing water and the first solution to produce a treatment solution;
Applying the treatment solution to the surface of a transparent substrate, and then drying the coated substrate;
The above-mentioned coating method including various steps. The method of claim 1 , wherein p + q> 8 and R is CH ₃ — or CH ₃ CH ₂ —. The method of claim 1, wherein the organosilane mixed into the first solution is 1H, 1H, 2H, 2H-perfluorodecyltriethoxysilane. Organosilane is mixed into the first solution, IH, IH, 2H, 2H-perfluorodecyl triethoxysilane, octadecyl triethoxysilane,及 beauty selected from the group consisting of mixtures thereof, The method of claim 1, wherein. Processing solution,
0 . An organosilane having a concentration in the range of from 0.5 to 50 mmol / liter ;
0 . A first solvent of water at a concentration ranging from 1 to 90% by weight ;
0 . At concentrations ranging from 5 to 20 wt%, and a second solvent selected ethylene bridging recall, glycerol, and mixtures thereof,
A third solvent selected from the group consisting of ethanol, propanol, butanol, and mixtures thereof;
The method of claim 1, comprising: The processing solution is 0 . The method according to claim 5 , comprising an organosilane in a concentration ranging from 1 to 10 mmol / l. The first solution contains 1H, 1H, 2H, 2H-perfluorodecyltriethoxysilane, isopropanol, water and an acid catalyst in a relative molar ratio of 1 : 1300: 11: 290, and the second solution contains water, Containing ethylene glycol and isopropanol in a relative molar ratio of 56000: 1500: 15000,
The method of claim 1. Also reacted for 2 hours and less first solution, the process of claim 1. The method of claim 1, wherein applying comprises immersing the substrate in a processing solution and then lifting the substrate from the processing solution. The step of withdrawing the substrate from the processing solution includes the steps of : The method according to claim 9 , wherein the method is performed at a speed of 001 cm / sec or more. The step of drying the coated substrate comprises:
Initially, the coated substrate is Drying in air, then followed and Drying at elevated temperature the coated substrate,
The method of claim 1, comprising steps. 2 0 min period of performed also coated substrate and least the step of drying initially; Moreover, drying subsequently the coated substrate is carried out a period of 2 0 minutes and less, The method of claim 11. The step of initially drying the coated substrate is performed at a temperature in the range of 10 to 40 ° C; and the step of subsequently drying the coated substrate is performed at a temperature in the range of 50 to 250 ° C. Item 12. The method according to Item 11 . The method of claim 11 , wherein the subsequent drying of the coated substrate is performed in an environment having a humidity in the range of 15-95%. 15. The method of claim 14 , wherein the subsequent drying of the coated substrate is performed in an environment having a humidity in the range of 40-80%. The method of claim 1, further comprising the step of aging the treatment solution for a plurality of days before using the treatment solution in the applying step. 17. The method of claim 16 , further comprising, after the aging step, adding an additional amount of the first solution to the processing solution. The method according to claim 1, wherein the substrate used in the applying step includes a material having a metal component or an inorganic component. 19. The method of claim 18 , wherein the substrate used in the application step comprises a polymethylmethacrylate substrate having an inorganic non-reflective coating. A method of applying an antifouling, hydrophobic optical coating to a transparent substrate,
Essentially, organosilane, an alcohol, a first solution having containing water and an acid catalyst to prepare,
The organosilane mixed in the first solution is represented by the following formula:
_{(RO) 3-n -Si- {} [C p + q H 2p F 2q] - (CH 3 Or -CF ₃ ) ｝ _{1 + n}
Wherein n is 0 to 3, p + q ≧ 2, and R is an alkyl group.
1H, 1H, 2H, 2H-perfluorodecyltrichlorosilane,
Octadecyltrichlorosilane, and
Selected from the group consisting of mixtures thereof,
Reacting the first solution for at least 2 hours;
Mixing a second solution containing a solvent selected from the group consisting of water, ethylene glycol, glycerol, ethanol, propanol, butanol, and mixtures thereof;
Mixing the first solution with the second solution to produce a processing solution;
The processing solution on the surface of the transparent substrate having a non-reflective coating of the inorganic and dip coating, and then the coated substrate in an environment having a humidity range of 15-95%, to Drying at elevated temperatures,
The above-mentioned coating method including various steps. A method of applying an antifouling, hydrophobic optical coating to a transparent substrate ,
0 . The following equation for a concentration in the range of 1 to 10 mmol / l
_{(RO) 3-n -Si- {} [C p + q H 2p F 2q] - (CH 3 Or -CF ₃ ) ｝ _{1 + n}
Wherein n is 0 to 3, p + q ≧ 2, and R is an alkyl group.
1H, 1H, 2H, 2H-perfluorodecyltrichlorosilane,
Octadecyltrichlorosilane, and
An organic silane selected from the group consisting of mixtures thereof ;
A first solvent of water at a concentration ranging from 0.1 to 90% by weight;
0. selected from the group consisting of ethylene glycol, glycerol, and mixtures thereof; A second solvent at a concentration ranging from 5 to 20% by weight;
A third solvent selected from the group consisting of ethanol, propanol, butanol, and mixtures thereof;
An acid catalyst;
Preparing a processing solution consisting essentially of:
Applying the treatment solution to the surface of a transparent substrate;
Drying the coated substrate;
The above-mentioned coating method including various steps. Organosilanes, IH, IH, 2H, 2H-perfluorodecyl triethoxysilane, octadecyl triethoxysilane,及 beauty selected from the group consisting of mixtures thereof, The method of claim 21, wherein. The step of drying the coated substrate comprises:
Initially, the coated substrate is Drying in air, then followed and Drying at elevated temperature the coated substrate,
22. The method of claim 21 comprising steps. 2 0 min period of performed also coated substrate and least the step of drying initially; Moreover, drying subsequently the coated substrate is carried out a period of 2 0 minutes and less, The method of claim 23. The step of initially drying the coated substrate is performed at a temperature in the range of 10 to 40 ° C; and the step of subsequently drying the coated substrate is performed at a temperature in the range of 50 to 250 ° C. Item 24. The method according to Item 23 . 24. The method of claim 23 , wherein the subsequent drying of the coated substrate is performed in an environment having a humidity in the range of 40-80%. A transparent substrate having an antifouling, hydrophobic, optical thin film coating applied using the method of claim 1.