KR102019315B1 - Method for super-hydrophobic coating - Google Patents

Abstract

The present invention relates to a method capable of forming a surface exhibiting super water-repellent properties based on a phenomenon that lamellar materials formed through hydrolysis reaction and self-assembly of hydrophobic silane chlorides in a specific solvent are coated on two-dimensional and three-dimensional surfaces. Especially, very uniform hydrophobic surface can be formed under acetone solvents in a concentration range of 2% and primarily on surfaces with hydrophobic properties, and the surface formed exhibits properties that exhibit a contact angle of at least 150 degrees.

Description

Surface formation method with super water-repellent property {Method for super-hydrophobic coating}

The present invention relates to a method of forming a surface having super water-repellent properties using a solution of silane compounds.

Superhydrophobic phenomenon refers to the property that water droplets bounce off rather than adhere to the surface. Surfaces with super water-repellent properties can be applied to various industrial fields because of their stain resistance and self-cleaning properties. In particular, the present invention can be applied for the purpose of solving safety and economic problems caused by freezing. For example, in the case of a transmission line, the load of the transmission line is greatly increased due to the icing of the surface of the transmission line in a cold area, a risk due to the loss and cutting of the transmission line and a safety problem due to the falling of ice. In addition, when such a problem occurs, a lot of time and money are required for recovery. When snow accumulates on the surface of the solar cell in winter, the absorption of solar light is inhibited, which causes problems of deterioration of the efficiency of the solar cell and cost and effort for removing the snow. It is necessary to utilize the technique of forming a transparent surface that does not impede passage.

In addition, in the refrigerant circulation part, which is an essential part of the refrigerator, the freezing efficiency is greatly reduced due to the ice formed due to condensation of the surrounding moisture due to the low temperature. Therefore, if the surface having super water-repellent properties can be made in an economical way, Applied to the above fields will be a way to solve the safety and economic problems will be a very useful technology industrially.

As a method for producing a surface having superhydrophobic characteristics, a method of modifying a surface having a hydrophobic group such as -CH ₃ , -CF _3, etc., which can lower surface energy, into a monomolecular layer or a multimolecular layer is known. However, the chemical surface modification method does not have sufficient water repellency (water contact angle of 150 degrees or less) and also has a disadvantage of low durability. A method of mimicking the micro-nanostructure of the lotus leaf surface, which shows excellent water repellent properties, has been proposed, and it is known that not only chemical surface treatment but also the formation of micro-nanostructure is necessary to construct a surface having super water-repellent properties with a contact angle of 150 degrees or more. have.

In order to form such a micro-nano structure, various sophisticated lithography methods and template-based methods used in semiconductor processes have been reported. There has been reported a method of producing a surface exhibiting a high water repellent property of water contact angle of 160 degrees or more by simultaneously applying a method of forming a nanomicro structure and hydrophobic surface treatment.

However, the method of forming the nanomicro structure, which is dependent on the semiconductor process, is not suitable for the surface structure forming method to impart super water-repellent property to a structure having a large area of several centimeters or more, and is particularly suitable for the surface of a curved material rather than a plane. Formation of the structure is impossible.

Therefore, chemical surface modification is mainly used as a method of forming a super water-repellent surface that is easy to apply to a large area of several cm or more. For example, a method of treating a silane compound having a low hydrophobic group with low surface energy has been reported. However, since the surface formed by such a method is composed of a monomolecular layer of hydrophobic groups, water repellency is insufficient and long-term durability is weak. An example of using a method of attaching nanoparticles dispersed in a solution to a surface to form a surface of super water-repellent properties by forming a nanomicro structure and using a hydrophobic surface group has been reported. Synthesis of an organic binder on nano silica particles such as Korean Application No. 10-2015-0049976 or Korean Patent Application Publication No. 10-2015-0059879 provides a super water-repellent coating surface and freezing durability by attaching a silane group having a low surface energy. The method of obtaining is known. In addition, Korean Patent Laid-Open Publication No. 10-2015-0054556 has also been reported a method of improving the characteristics by coating after chemical and thermal pretreatment for aluminum adsorbent to improve water repellency and icing durability. However, as a method of attaching the nanoparticles to the surface, it is known that the nanoparticles are uniformly attached to a wide surface or curved surface of several cm or more.

1997 J. Am. Chem. According to the Soc paper (J. Am. Chem. Soc. 1997, 119, 3135-3143), plate crystals can be formed in aqueous solution through the hydration of 18 carbon silane chloride (n-octadecyltrichlorosilane) in distilled water. I've seen it.

In 2010, Langmuir's paper (2010, 26 (5), pp 3579-3584) first prepared a substrate on which the n-octadecyltrichlorosilane reagent with viscosity on the glass surface was first prepared, and then n-octa A method of forming a surface of super water-repellent property through a polymerization reaction through hydration of n-octadecyltrichlorosilane and cross reaction of siloxane on the surface of the substrate by dipping the decyltrichlorosilane-coated substrate into acetone solvent. I have reported. In 2010, ACS applied materials & interface journal immersed 1-5 times the surface to give super water-repellent properties to ethanol solution of silica nanoparticles and n-octadecyltrichlorosilane, dried in air, oven (45 degrees) The method of preparing a surface exhibiting super water-repellent properties by a final drying method has been presented. However, this conventional method is a method of coating the substrate with a viscous n-octadecyltrichlorosilane and then forming a white plate crystal through the hydrolysis reaction and polymerization reaction, so that the coating layer on the substrate surface is uniform. It has a disadvantage in that the transmittance in visible light is very low.

A. N. Parikh, et al., Journal of the American Chemical Society. 1997, vol. 119, issue 13, 3135-3143 Qingping Ke, et al., Langmuir, 2010, vol. 26, issue 5, 3579-3584 Qingping Ke, et al., ACS applied materials & interface, 2010, vol. 2, issue 8, 2393-2398

It is an object of the present invention to provide a method for producing a surface that exhibits super water repellent properties uniformly on a surface of various materials with a large area of several cm or more.

Item 1. A composition for water repellent coating comprising alkyl (C12-25) trichlorosilane dissolved in dialkyl (C2-6) ketone.

Item 2. The composition of item 1, wherein the dialkyl (C 2-6) ketone is acetone.

Item 3. The composition of item 2, wherein the acetone contains at least 1% (v / v) and less than 5% (v / v) moisture.

Item 4. The composition of item 1 or 2, wherein the alkyl (C12-25) trichlorosilane is n-octadecyltrichlorosilane.

Item 5. The composition of item 1 or 2, wherein the alkyl (C12-25) trichlorosilane is comprised between 1% (v / v) and 3% (v / v) relative to the dialkyl (C2-6) ketone.

Item 6. Dipping the substrate to be coated in the dialkyl (C2-6) ketone, and dissolving the alkyl (C12-25) trichlorosilane in the dialkyl (C2-6) ketone in which the substrate is immersed. Or dissolving an alkyl (C12-25) trichlorosilane in a dialkyl (C2-6) ketone, and immersing the substrate to be coated in the solution.

Item 7. The method according to item 6, wherein the dialkyl (C 2-6) ketone is acetone.

Item 8. The method of item 7, wherein the acetone contains at least 1% (v / v) and less than 5% (v / v) water.

Item 9. The method according to item 6 or 7, wherein the alkyl (C12-25) trichlorosilane is octadecyltrichlorosilane.

Item 10. The process according to item 6 or 7, wherein the alkyl (C12-25) trichlorosilane is dissolved from 1% (v / v) to 3% (v / v) relative to the dialkyl (C2-6) ketone. .

Item 11. The method according to item 6 or 7, wherein the substrate has a hydrophobic surface or a hydrophilic surface.

Item 12. The method according to item 6 or 7, wherein the substrate is immersed in the solution for at least 30 minutes.

Item 13. Articles coated by the method according to item 6 or 7.

Item 14. The article of item 13, wherein the surface of the coated article has a contact angle of at least 150 ° at 25 ° C. with respect to water.

Item 15. The article of item 13 or 14, wherein the coating has a light transmittance of at least 50%.

When applying the method according to the invention it is possible to produce a uniform super water-repellent surface regardless of the shape of the surface, regardless of the shape of the surface, regardless of the material of the glass surface, the metal surface, the surface of the plastic surface to be coated, The formed superhydrophobic surface has a contact angle of water of at least 150 degrees and exhibits visible light transmittance of at least 50%. The super water-repellent surface thus formed has an effect of suppressing icing and further suppressing freezing.

1 is a coating composition (FIG. 1A) according to an embodiment of the present invention, a coating method using the composition (FIG. 1B), a coated article (FIG. 1C), and an image of the surface thereof taken with an electron scanning microscope (FIG. 1D). )to be.
Figure 2 is a photograph of the self-assembly of the moisture content and time after the OTS-Cl injection.
Figure 3 is the silane to the embodiment 2 (w / v)% of octadecyl trichloro according to the invention with a silane, respectively (n -octadecyltrichlorosilane OTS), a silane-dodecyl-trichloroethane, trichloro silane, octyl, butyl and trichloroethyl It is a photograph dissolved in toluene, acetone and water solvent.
4 is octanoic tilt Rie silane according to one embodiment of the invention the surface of a glass substrate coated with acetone, toluene, and ethanol solution;; (OTS n -octadecyltrichlorosilane) ( octyltriethoxysilane OTES) and octadecyl trichlorosilane by Was analyzed by an Atomic Force Microscope (AFM) image (FIG. 4A), X-ray photoelectron spectroscopy (XPS) analysis (FIG. 4B) and contact angle measurement (FIG. 4C). )to be.
FIG. 5 shows the results of observing the self-assembled octadecyltrichlorosilane in a solution in which octadecyltrichlorosilane was dissolved in acetone using an electron scanning microscope (FIG. 5A), FT-IR analysis result (FIG. 5B), and Raman analysis result ( 5C).
FIG. 6 is an AFM photograph of a surface coated with an octadecyltrichlorosilane-acetone solution on a hydrophilic surface (FIG. 6A) and a hydrophobic surface (FIG. 6B), and confirmed transparency.
FIG. 7 shows the results of high-speed imaging, respectively, when water was dropped on a plate having a hydrophobic surface inclined at 30 ° at −25 ° C. (FIG. 7A) and a plate coated with octadecyltrichlorosilane (FIGS. 7B and 7C). .
FIG. 8 is an image photographing a result of coating a large area, a curved surface, and surfaces of various materials with 2% octadecyl trichlorosilane in an acetone solution.

The invention will now be described more fully hereinafter with reference to the accompanying drawings. However, only some embodiments of the present invention are illustrated. Indeed, these inventions may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. As used in this specification and the appended claims, the singular forms “a,” “an” and “the” include plural referents unless the context clearly dictates otherwise.

In order to produce a surface exhibiting super water-repellent properties (surface properties exhibiting a water contact angle of more than 150 degrees), surface modification using a compound having a hydrophobic functional group with nanomicro level surface curvature is essential. In the current semiconductor process, such as e-beam lithography (lithography), it is very economical to form a nano-microscopic surface structure in a large area of several cm or more, it is very difficult to commercialize. A simple chemical surface modification method cannot achieve super water-repellent properties of water contact angles of more than 150 degrees. Although it is possible to attach to the surface to achieve super water-repellent properties by using a solution in which nanoparticles are easily applied to a larger area, it is also a method to attach nanoparticles evenly to curved surfaces. .

Therefore, the present inventors have attempted to overcome the above problems and to attempt a surface treatment method that exhibits a uniform superhydrophobic property in a large area irrespective of the material and shape of the surface to implement superhydrophobic characteristics, and the results of repeated studies In a single solution surface treatment process, nanomicro structure and hydrophobic properties are given to the surface of a large area to develop a method capable of producing a surface exhibiting super water repellent properties.

In order to form a hydrophobic surface on the glass surface, a trialkoxysilane-based compound is mainly applied to a surface having a hydroxyl group and used to form a transparent surface of hydrophobic property through siloxane bonds. However, this simple chemical surface modification method does not exhibit super water-repellent properties of water contact angle of more than 150 degrees. The present inventors tried to form a hydrophobic surface with n-octadecyltriethoxysilane and n-octadecyltrichlorosilane to form a hydrophobic surface on the glass surface, but n-octadecyl Triethoxysilane did not produce crystals through hydration and self-assembly in acetone, toluene, ethanol and the like, and n-octadecyltrichlorosilane did not form crystals through self-assembly under toluene and ethanol solvents. However, in particular, n-octadecyltrichlorosilane does not form crystals within a few hours in acetone solvents containing less than 0.1% water, whereas acetone containing more than 0.1% water can undergo crystallization through hydration and self-assembly. Found to be produced.

In particular, when pure distilled water is used as a solvent, crystals formed through hydration and self-assembly of n-alkyltrichlorosilane are found to have rods, spheres, and plates according to the carbon number of the alkyl group. When this is applied to the surface, since no uniform surface coating is applied, pure distilled water is an undesirable solvent for forming a superhydrophobic surface.

Dialkyl (C2-6) ketone means a dialkyl ketone having 2 to 6 carbons. In the present invention, a dialkyl (C2-6) ketone solvent may be used, but C2 (acetone) Is most preferred.

However, while the amount of water in the acetone ranges from 0.1% to 5% (v / v), the concentration of n-octadecyltrichlorosilane is 0.1-4% (v / v), more preferably 1 The case of -3% (v / v), and most preferably 2% (v / v), showed a uniform water repellency and uniform thickness of the coating layer.

When the water content in the acetone solvent is less than 0.1%, the hydration reaction of n-octadecyltrichlorosilane is slow, and formation of a crystal structure through self-assembly is not preferable. In addition, when the moisture in the acetone solvent exceeds 5%, the surface coating is not uniform, which is not preferable.

A plate-like lamellar structure having a thickness of 1-10 microns is formed on the glass surface, but a plate-like lamellar structure having a thickness in the range of 1-5 microns is more preferable, wherein the visible water transmittance is 50% or more, and the water repellency of 150 degrees or more is super water-repellent. It was confirmed that the characteristics appear.

When the number of carbon atoms of the n-alkyltrichlorosilane hydrophobic group (R) is less than 12, no crystal structure is produced through self-assembly in an acetone solvent. Thus, the number of carbon atoms of the hydrophobic group in the n-alkyltrichlorosilane is preferably 12 or more. The present invention relates to a composition for water repellent coating comprising alkyl (C12-25) trichlorosilane dissolved in dialkyl (C2-6) ketone. It relates to a composition for water repellent coating comprising octadecyltrichlorosilane. Unlike toluene as a conventional solvent, the present invention uses dialkyl ketone as a solvent. Preferably alkyl in the dialkyl (C2-6) ketone may be each independently alkyl of 1 to 5 carbon atoms, more preferably each independently methyl, ethyl, propyl, butyl, isopropyl, pentyl, isopentyl and neo At least one selected from pentyl, most preferably the dialkylketone is acetone.

The alkyl (C12-25) trichlorosilane means an alkyl having 12 to 25 carbon atoms, preferably octadecyltrichlorosilane (octadecyltrichlorosilane). The octadecyltrichlorosilane includes about 1% (v / v) to about 3% (v / v), or about 2% (v / v) with respect to the dialkyl ketone, but is not limited thereto. no.

The method of coating a substrate with octadecyltrichlorosilane according to the present invention will be described in detail with reference to FIG. 1. Immersing the substrate in a dialkyl ketone in one embodiment of the present invention; And mixing octadecyltrichlorosilane with dialkyl ketone on which the substrate is immersed, or mixing octadecyltrichlorosilane with dialkyl ketone; And it provides a method of water-repellent coating the substrate, comprising the step of immersing the substrate in the solution. In one embodiment, the dialkyl ketone may be acetone, and the octadecyltrichlorosilane is about 1% (v / v) to about 3% (v / v), or about 2, relative to the dialkyl ketone Included as% (v / v), but not limited to. In acetone, 2 v / v% octadecyl trichlorosilane in; when dissolving the (n -octadecyltrichlorosilane OTS) octadecyl silane (octadecyltrichlorosilane) trichlorosilane is hydrolyzed to cross-linking is self-assembled after condensation (polycondensation) lamellar nano It will form a sheet or nano-square plate, it is possible to create a super water-repellent surface by increasing the surface roughness, contact angle and surface tension. When water is dropped onto the coated surface according to the present invention, the water droplets come into contact with the vertices of the super water-repellent surface having the nanostructure, while the water droplets do not penetrate below the vertices, thereby minimizing the hydrophobicity by minimizing the contact area between the water and the surface. Will be displayed.

The water-repellent coating method according to the present invention can be coated irrespective of whether the surface of the substrate to be coated is hydrophilic or hydrophobic, and can be coated regardless of whether the surface is flat or uneven, and can be applied over a large area. There is an advantage that it can. The substrate to be coated may be, for example, glass, polyurethane, wood, plastic, fiber or metal, but is not limited thereto. Preferably the substrate has a hydrophobic surface.

The process according to the present invention is characterized in that the coating is simply immersed in an acetone-octadecyltrichlorosilane solution for about 30 seconds, about 1 minute, about 10 minutes, about 30 minutes, about 1 hour or about 2 hours or longer. It is possible.

The surface of the article coated according to the method of the present invention has a lamellar nanosheet shape, the contact angle with respect to water at 25 ℃ can be 150 ° or more, and is coated to a thickness in the range of 1 to 10 micro or 1 to 5 micro, The cotton may have a light transmittance of about 50% or more.

Contact angle means the angle between the liquid and solid surface. In one embodiment of the present invention, the contact angle is measured using a Kruess contact angle measurement system G100 measuring device equipped with a CCD camera. The advancing contact angle and the receding contact angle are respectively measured while the droplets grow and shrink. The static contact angle is measured in the sessle drop state. Sliding angle is measured by the angle at which water droplets begin to flow on the surface.

Fourier-transform infrared spectroscopy (FT-IR) is an analysis method that analyzes the molecular vibration mode in the infrared region and analyzes the properties of the measurement sample. Measure the absorption of energy corresponding to rotation.

Raman analysis is a spectroscopic method used to measure vibrations, rotations, and other low frequency conditions in a system. It mainly uses a single wavelength of light in the visible, near-infrared, or near-ultraviolet region produced by a laser, and inelastic collisions. Depends on scattering or Raman scattering.

In one embodiment of the present invention the coating surface was observed by X-ray photoelectron spectroscopy (XPS). XPS data was collected with an Escalab 250 probe system with an aluminum cathode. The diameter of the X-ray spot was about 500 μm, and the equipment was equipped with a spherical capacitor energy analyzer (SCEA) and a multichannel detector. High resolution scan C 1s (278-298 eV) was collected after surface irradiation scan.

Hereinafter, the present invention will be described with reference to specific examples. The following examples are intended for illustrative purposes only and are not intended to limit the scope of the invention in any way.

Example 1. Octadecyltrichlorosilane super water-repellent coating with acetone (water less than 0.01% (v / v)) as a solvent

Acetone with 99% purity was warmed and distilled. Molecular sieve was added to the distilled acetone to completely remove water, and 1 L of acetone adjusted to less than 0.1% of water in acetone was placed in a beaker, and a super water-repellent surface coating was applied. The glass substrate to be formed was immersed. 20 g of n -octadecyltrichlorosilane was quickly added to the solution and shaken. Crystallization and self-assembly at room temperature were expected to produce crystals and adhere to the surface of the glass substrate, but crystals did not precipitate even after 1 hour. FIG. 2 is a solution photograph of 2% n-octadecyltrichlorosilane added to acetone with less than 0.1% moisture, and crystals do not form as shown in the photograph after 10 seconds and 1 hour after adding n-octadecyltrichlorosilane. can confirm.

Example 2. Octadecyltrichlorosilane super water-repellent coating with acetone (adjusted to about 0.1-1% (v / v) moisture) as a solvent

99% pure acetone was heated and distilled, and molecular sieve was added to the distilled acetone to completely remove water, and 1 L of acetone adjusted to 0.5% water in acetone was placed in a beaker, forming a super water-repellent surface coating. The glass substrate to be immersed. 20 g of octadecyltrichlorosilane ( n -octadecyltrichlorosilane) was quickly added to the solution and shaken. After 1 hour, the substrate coated with a white translucent surface was washed with acetone and dried at room temperature.

n - after mixing with octadecyl trichloro silane in acetone and water 0.5% (v / v) for about 10 seconds n -octadecyltrichlorosilane the hydration and the self-assembly it was confirmed that the white solid formed in the solution. (See Figure 2). In addition, about 30 minutes after the white precipitate occurred, a super water-repellent surface was formed.

Example 3. Octadecyltrichlorosilane super water-repellent coating using acetone (moisture 5.0% (v / v) or more) as a solvent

99% pure acetone was heated and distilled, and molecular sieve was added to the distilled acetone to completely remove water, and 1 L of acetone adjusted to 6.0% of water in acetone was placed in a beaker, forming a super water-repellent surface coating. The glass substrate to be immersed. 20 g of octadecyltrichlorosilane ( n -octadecyltrichlorosilane) was quickly added to the solution and shaken. After 1 hour, the substrate coated with a white translucent surface was washed with acetone and dried at room temperature.

n - is after about 10 seconds, n- octadecyl trichloro silane hydration and self-assembled after mixing the silane with octadecyl trichloro in acetone in water 6.0% (v / v) were formed in the solution a white solid. (FIG. 2) In addition, although a super water-repellent surface was formed on the substrate immersed for 30 minutes or more after the white precipitate occurred, a large amount of grains of 0.5 to 1 mm were present on the surface, and the surface was not uniform. Coating.

As a result of comparing Examples 1 to 3, it was confirmed that acetone having a water content of 0.1-1.0% (v / v) was the most suitable solvent for super water-repellent coating using n -octadecyltrichlorosilane.

Example 4 Self-Assembly Structure Generation Experiment in Toluene Solvent of Alkyltrichlorosilane

20 g of octadecyl trichlorosilane, dodecyl trichlorosilane, octyl trichlorosilane and butyl trichlorosilane were rapidly added to 1 L of toluene and shaken. After immersing the glass substrate for 30 minutes, 1 hour, 2 hours, 3 hours, 5 hours, 8 hours, and 12 hours, respectively, the coated substrate was washed with acetone, dried at room temperature, and then a superhydrophobic surface was formed. Confirmed.

When octadecyltrichlorosilane, dodecyltrichlorosilane, octyltrichlorosilane and butyltrichlorosilane were used as the solvent, no observable precipitation occurred in all cases. (FIG. 3A).

Example 5 Self-Assembly Structure Generation Experiment in Distilled Water Solvent of Alkyltrichlorosilane

20 g of octadecyl trichlorosilane, dodecyl trichlorosilane, octyl trichlorosilane and butyl trichlorosilane were quickly added to 1 L of distilled water and shaken.

As a result, within 10 seconds, a observable precipitation was produced in all cases. When octadecyltrichlorosilane and dodecyltrichlorosilane were used as in the electron micrograph of FIG. 3, a plate-shaped crystal structure was produced, but when the octyltrichlorosilane was used, spherical particles were formed. Butyltrichlorosilane was confirmed to form a rod-shaped crystal structure. This rapid reaction and formation of amorphous precipitates were judged to be unsuitable for use as a method of forming a uniform super water-repellent coating surface (FIG. 3C).

Example 6 Self-Assembly Structure Generation Experiment in Acetone Solvent of Alkyltrichlorosilane

20 g of octadecyltrichlorosilane, dodecyltrichlorosilane, octyltrichlorosilane and butyl trichlorosilane were rapidly added to 1 L of acetone having a water content of about 2%, and shaken.

As a result, an observable precipitate was produced when using n-octadecyltrichlorosilane after about 30 seconds. When dodecyltrichlorosilane was used, a white precipitate formed after about 5 hours, but no precipitation was produced when octyltrichlorosilane and butyltrichlorosilane were used (FIG. 3B).

Example 7 Superhydrophobic Coating with Octadecyltriethoxysilane and Octadecyltrichlorosilane in Acetone, Toluene, and Ethanol Solvents

Acetone, toluene, and 1 L of ethanol were each placed in a beaker to immerse the transparent glass substrate. 20 g of octadecyltriethoxysilane and octadecyltrichlorosilane were quickly added to each of the solutions on which the glass substrate was immersed and shaken.

When octyltriethoxysilane was used, substantially no coating was made (2-4 in FIGS. 4A, 4B, and 4C), and acetone (FIGS. 4A, 4B, 4) was used when octadecyltrichlorosilane was used. And superhydrophobic coating was formed only in 5) solvent of FIG. 4C. When toluene and ethanol solutions were used, no effective coatings were also produced in octadecyltrichlorosilane (FIGS. 4A, 4B, and 6 and 7 of FIG. 4C).

In combination with Examples 1 to 7, it can be seen that the super water-repellent coating can be formed when octadecyltrichlorosilane is used in 1 L of acetone having a water content of about 2%.

Example 8. Physicochemical Properties of Octadecyltrichlorosilane in Acetone Solvent

As a result of observing the top, middle, and bottom of the super water-repellent coating solution prepared according to Example 2 with an electron scanning microscope, a nano-square plate was formed on the top of the solution, and a lamella on the bottom. It was confirmed that a structure was formed (FIG. 5A). In addition, FT-IR analysis results (FIG. 5B) and Raman analysis results (FIG. 5C) supported that octadecyltrichlorosilane forms nano-square plates and lamellar structures.

Example 9 Superhydrophobic Coating of Substrates with Hydrophilic Surfaces and Substrates with Hydrophobic Surfaces

A glass surface having a hydrophilic surface and a glass surface modified to have a hydrophobic surface by treating toluene and octadecyltrichlorosilane on the glass were coated according to Example 2, and the surface of the coated substrate was subjected to atomic force microscopy; AFM).

As a result, the three-dimensional solid lamellar structure was confirmed in both the substrate having a hydrophilic surface (FIG. 6A) and the substrate having a hydrophobic surface (FIG. 6B), and was expected to exhibit superhydrophobic properties. It was also confirmed that both had light transmittance of 50% or more.

Example 10 Identification of Icephobic Properties and Surface Properties

Water was applied at a height of 10 cm on a glass substrate modified to have a hydrophobic surface by treating toluene and octadecyltrichlorosilane, inclined at 30 ° at -25 ° C, and a substrate coated with octadecyltrichlorosilane on a hydrophilic surface and a hydrophobic surface I dropped a drop. High-speed shooting was performed from the moment of dropping the water droplets (FIG. 7), and the radius of the water droplets (spreading) and the remaining water on the substrate when the radius of the water droplets reaches the plate (impact) and the radius of the water droplets are the largest. The radius of the water droplet (contraction) was measured. The shape and movement of the water droplets were observed after the contraction, and the results are shown in Table 1 and FIG. 7.

Board Hydrophobic substrate
(FIG. 7A) Hydrophilic Surface + Octadecyltrichlorosilane Coated Substrate
(FIG. 7B) Hydrophobic Surface + Octadecyltrichlorosilane Coated Substrate
(Figure 7C) impact 3 mm 2.7 mm 2.9mm Spreading 9.15mm 7.04mm 7.14 mm Contract 1.55 mm 1.1mm 0 mm

As described in Table 1 and FIG. 7, when the hydrophilic surface and the hydrophobic surface were coated with octadecyltrichlorosilane, high water repellency was observed, and as a result, it was confirmed that icing and freezing could be effectively suppressed.

Example 11. Large Area Super Water Repellent Surface Formation and Super Water Repellent Surface Formation in Various Materials

In order to confirm that the method of acetone solution of 2% octadecyltrichlorosilane is applicable to a large area of several inches or more, the surface of 6 inches of glass is immersed in acetone solution of 2% octadecyltrichlorosilane for 1 hour. The state was confirmed. As shown in Figure 8 it was confirmed that a white uniform surface can be formed in a large area of 6 inches.

Furthermore, the same method was applied to glass vials, glass tubes, and the like in order to confirm that not only the flat glass surface but also the inner and outer surfaces of the curved glass can form super water-repellent surface. As shown in FIG. 8, white uniform surfaces were formed inside the glass vial and outside the glass tube.

In addition, the same method was applied not only to the surface of glass but also to various surface materials in order to confirm the formation of super water-repellent surface in the same way. As confirmed in FIG. 8, it was confirmed that a white uniform coating was formed on the copper tube surface and the polyurethane surface.

For example, for purposes of claim construction, the claims set forth below should not be construed in any way narrower than their literal language, and therefore, illustrative embodiments from the specification should not be read as claims. Accordingly, it is to be understood that the invention has been described by way of example and not as limitations on the scope of the claims. Accordingly, the invention is limited only by the following claims. All publications, published patents, patent applications, books, and journal articles cited in this application are hereby incorporated by reference in their entirety.

Claims (15)

A water repellent coating composition comprising alkyl (C12-25) trichlorosilane dissolved in a dialkyl (C2-6) ketone, wherein the dialkyl (C2-6) ketone is acetone and the acetone is 1% (v / v) and at least 5% (v / v) moisture. The composition of claim 1, wherein the alkyl (C12-25) trichlorosilane is n-octadecyltrichlorosilane. The composition of claim 1, wherein the alkyl (C 12-25) trichlorosilane is comprised between 1% (v / v) and 3% (v / v) relative to the dialkyl (C 2-6) ketone. Immersing the substrate to be coated in the dialkyl (C2-6) ketone, and
Or dissolving the alkyl (C12-25) trichlorosilane in the substrate-immersed dialkyl (C2-6) ketone,
Dissolving alkyl (C12-25) trichlorosilane in dialkyl (C2-6) ketone, and
A method of water repellent coating a surface of a substrate, comprising immersing a substrate to be coated in the solution, wherein the dialkyl (C2-6) ketone is acetone, and the acetone is at least 1% (v / v) and 5 containing less than% (v / v) moisture. The method of claim 4, wherein the alkyl (C12-25) trichlorosilane is octadecyltrichlorosilane. The method of claim 4, wherein the alkyl (C 12-25) trichlorosilane is dissolved at 1% (v / v) to 3% (v / v) relative to the dialkyl (C 2-6) ketone. The method of claim 4, wherein the substrate has a hydrophobic surface or a hydrophilic surface. The method of claim 4, wherein the substrate is immersed in the solution for at least 30 minutes. An article coated by the method according to claim 4. The article of claim 9, wherein the surface of the coated article has a contact angle of at least 150 ° at 25 ° C. with respect to water. The article of claim 9, wherein the coating has a light transmittance of at least 50%. The article of claim 9, wherein the coating is 1-10 μm thick. delete delete delete

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