CN111471330A - Hydrophilic-hydrophobic transparent coating with adjustable surface roughness and preparation method thereof - Google Patents
Hydrophilic-hydrophobic transparent coating with adjustable surface roughness and preparation method thereof Download PDFInfo
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- CN111471330A CN111471330A CN202010162374.9A CN202010162374A CN111471330A CN 111471330 A CN111471330 A CN 111471330A CN 202010162374 A CN202010162374 A CN 202010162374A CN 111471330 A CN111471330 A CN 111471330A
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
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Abstract
The invention discloses a hydrophilic and hydrophobic transparent coating with adjustable surface roughness and a preparation method thereof. The transparent coatings with different hydrophilicity and hydrophobicity can be obtained by adjusting the adding amount of siloxane or fluorosilane reagent, and the transparent coatings with different roughness can be obtained by adjusting the mixing ratio of the suspension and the absolute ethyl alcohol. In summary, the preparation method can simultaneously adjust the surface wettability and roughness of the transparent coating, so that the obtained transparent coating can be changed from a super-hydrophilic state to a hydrophilic state, a hydrophobic state and a super-hydrophobic state. The method is simple to prepare and low in cost, and the obtained coating has diversified functions and can meet the surface application of materials with requirements on light transmittance, such as the surface of a photovoltaic panel, the surface of a building, a vehicle window and the like.
Description
Technical Field
The invention belongs to the field of super-hydrophobic materials, and particularly relates to a transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness and a preparation method thereof.
Background
In recent years, super-hydrophobic coatings or super-hydrophilic coatings have very good application prospects in production and life, and can realize multiple functions such as self-cleaning, oil resistance, pollution resistance, fog resistance, bacteriostasis and the like. The preparation methods of the super-hydrophobic and super-hydrophilic materials are very various, the technology is relatively mature, various preparation technologies usually obtain coating surfaces with different properties by changing the surface chemical properties and the coarse structure, and the common methods include an ion etching method, a layer-by-layer assembly method, a chemical etching method, a chemical vapor deposition method and the like. Although either superhydrophobic or superhydrophilic coatings can be obtained by different methods, coatings prepared by different methods often have different types of roughness (such as needle-like, spherical, irregular raised, etc.) or different chemical properties (such as fluorine, methyl, methylene, etc.). Even though these coatings all have the functions common to super-hydrophobic or super-hydrophilic coatings, such as self-cleaning, etc., different roughness structure types and chemistries add difficulties to our single-factor or two-factor experiments to investigate in depth how both quantitatively affect the process of achieving the self-cleaning, etc. functions. Therefore, the coating surface with the same rough structure and the same chemical property but with the roughness and the wettability capable of being regulated and controlled is prepared, and further theoretical research is facilitated. In addition, many of the hydrophobic or hydrophilic surfaces obtained by the preparation methods are non-transparent, which limits their application to materials requiring light transmittance, such as photovoltaic panels, architectural glass, vehicle windows, and the like.
Disclosure of Invention
In order to solve the problems and the defects in the prior art, the invention aims to provide a transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness and a preparation method thereof. The method can simultaneously regulate and control the roughness and the wettability of the surface of the material, so that the super-hydrophilic surface, the hydrophobic surface and the super-hydrophobic surface with the same rough structure and the same chemical properties but different roughness and different wettability are obtained, and meanwhile, the material has the transparent characteristic.
In order to achieve the above object, a first aspect of the present invention provides a hydrophilic-hydrophobic transparent coating with adjustable surface roughness, comprising the steps of:
(1) taking tetraethoxysilane, ammonia water and absolute ethyl alcohol as raw materials, mixing and stirring to prepare hydrophilic silica-soluble collagen liquid;
(2) uniformly mixing silicon-soluble collagen liquid and a siloxane reagent or a fluorosilane reagent, then adding silicon dioxide nano powder particles into the mixture, and uniformly stirring the mixture at normal temperature to obtain suspension;
(3) and (3) mixing the suspension with absolute ethyl alcohol, performing ultrasonic oscillation, and coating the mixture on the surface of a base material to form a film, thus obtaining the transparent super-coating, wherein the transparent super-coating has different hydrophilicity and hydrophobicity and different surface roughness according to different parameters of the steps (1) - (3).
Further setting the volume ratio of the ethyl orthosilicate, the ammonia water and the absolute ethyl alcohol in the step (1) to be 1:1: 35-1: 3:35, and stirring at the temperature of 30-60 ℃.
Further setting the silicon-soluble collagen solution obtained in the reaction of the step (1) to be light blue solution in which 20-50nm of silicon dioxide is uniformly dispersed.
It is further provided that the siloxane or fluorosilane reagent in the reaction of step (2) is any one of methyltriethoxysilane, methyltrichlorosilane, hexamethyldisilazane, trimethylchlorosilane, perfluorodecyltrimethoxysilane, tridecafluorooctyltrimethoxysilane, etc.
Further setting the size of the silicon dioxide nano powder added in the reaction in the step (2) to be 7-60 nm.
Further setting that the amount of the silica nanopowder added in the reaction of step (2) is 0.02g per 1ml of the silica-soluble collagen solution.
The volume ratio of the silica-soluble collagen solution to the siloxane reagent in the reaction of the step (2) is 1: 0-1: 0.1, and the wettability of the prepared transparent coating is gradually changed from super-hydrophilic to super-hydrophobic along with the sequential change of the ratio of the silica-soluble collagen solution to the siloxane reagent in the interval.
Further setting that the volume of the suspension taken out in the reaction in the step (3) is 75-800 mu L, and mixing the suspension with 1m L absolute ethyl alcohol, thereby preparing the transparent coating with the root-mean-square roughness varying from dozens of nanometers to hundreds of nanometers.
And (3) further setting that the substrate in the reaction in the step (3) is glass, plastic, a photovoltaic plate, a metal plate or a rubber plate, and the coating mode is a pulling method, a spin coating method or a spraying method.
In addition, the invention also provides the transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness, which is prepared by the preparation method.
The invention has the beneficial effects that:
the preparation technology related by the invention is simple, does not need complex equipment or precise instruments, and can obtain the coating surface with different roughness and wettability only by regulating and controlling the adding proportion of the reagent. The roughness of the coating prepared by the method can be changed from dozens of nanometers to hundreds of nanometers, the wettability can be gradually changed from super-hydrophilic to super-hydrophobic state, the purpose of regulating and controlling the surface roughness and wettability of the coating in a large width is realized, and convenience is provided for deeply and quantitatively researching the influence of the surface roughness and wettability on the coating function realization process. In addition, because the coatings are transparent and do not affect the appearance of the base material, the coatings can be flexibly applied to the surfaces of materials with requirements on light transmittance, such as photovoltaic panels, building glass, vehicle windows and the like according to actual functional requirements (such as a super-hydrophilic surface for obtaining an anti-fog function or a super-hydrophobic surface for obtaining a self-cleaning function and the like).
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is within the scope of the present invention for those skilled in the art to obtain other drawings based on the drawings without inventive exercise.
FIG. 1 values of light transmittance and contact angle for a blank glass and a superhydrophilic coating;
FIG. 2 light transmittance and contact angle values for a blank glass and a hydrophilic coating;
FIG. 3 light transmittance and contact angle values for a blank glass and a hydrophobic coating;
fig. 4 values of light transmittance and contact angle for the blank glass and the superhydrophobic coating.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
Example 1
Mixing tetraethoxysilane, ammonia water and absolute ethyl alcohol according to the volume ratio of 1:1.5:35, stirring for 10 hours at the temperature of 60 ℃ to obtain hydrophilic silicon-soluble collagen liquid, taking out 15ml of the silicon-soluble collagen liquid, adding into a beaker, adding 0.3g of silicon dioxide nano powder particles, stirring uniformly at the normal temperature to obtain suspension, taking out 300 mu L suspension, mixing with 1m L absolute ethyl alcohol, carrying out ultrasonic oscillation for 1 hour, and forming films on the surfaces of different base materials by using a pulling method.
The contact angle test, the roughness test and the light transmittance test were performed on the surface of the coating layer prepared by the above method, and the results are shown in fig. 1. As can be seen from the figure, the coating contact angle is 0 DEG, and the coating is in a super-hydrophilic state; the transmittance data of the coated glass and the blank glass at 800nm under 300-800nm are shown in figure 1, the transmittance of the coated glass is not reduced, but is slightly higher than that of the blank glass, and therefore, the coating obtained by the method is a transparent super-hydrophilic coating. The root mean square roughness of the coating surface is 74.1nm through surface roughness test.
Example 2
Mixing tetraethoxysilane, ammonia water and absolute ethyl alcohol according to the volume ratio of 1:1.9:35, stirring for 10 hours at the temperature of 30 ℃ to obtain hydrophilic silica-soluble collagen liquid, taking out 10ml of the silica-soluble collagen liquid and taking out 0.3ml of hexamethyldisilazane, uniformly mixing, then adding 0.2g of silicon dioxide nano powder particles, uniformly stirring at the normal temperature to obtain suspension, taking out 350 mu L suspension, mixing with 1m L absolute ethyl alcohol, carrying out ultrasonic oscillation for 1 hour, and forming films on the surfaces of different base materials by a spraying method.
The contact angle, roughness and transmittance of the coating surface prepared by the above method were measured, and the results are shown in fig. 2. As can be seen, the coating has a contact angle of 62.6 degrees and is in a hydrophilic state; the transmittance data of the coated glass and the blank glass at 300-800nm are shown in FIG. 2, and the transmittance of the coated glass is slightly higher than that of the blank glass, so that the coating obtained by the method is a transparent hydrophilic coating. The surface roughness test shows that the root mean square roughness of the coating surface is 88.9 nm.
Example 3
Mixing tetraethoxysilane, ammonia water and absolute ethyl alcohol according to a volume ratio of 1:2:25, stirring for 10 hours at 30 ℃ to obtain hydrophilic silica-soluble collagen liquid, taking out 10ml of the silica-soluble collagen liquid and 0.8ml of hexamethyldisilazane, uniformly mixing, then adding 0.2g of silicon dioxide nano powder particles, uniformly stirring at normal temperature to obtain a suspension, taking out 75 mu L suspension, mixing with 1m L absolute ethyl alcohol, ultrasonically shaking for 1 hour, and forming films on the surfaces of different base materials by using a spin coating method.
The contact angle, roughness and transmittance of the coating surface prepared by the above method were measured, and the results are shown in fig. 3. As can be seen from the figure, the coating has a contact angle of 113.5 ° and is in a hydrophobic state; the transmittance data of the coated glass and the blank glass at 300-800nm are shown in FIG. 3, and the transmittance of the coated glass is slightly higher than that of the blank glass, so that the coating obtained by the method is a transparent hydrophobic coating. The surface roughness test shows that the root mean square roughness of the coating surface is 30.8 nm.
Example 4
Mixing tetraethoxysilane, ammonia water and absolute ethyl alcohol according to the volume ratio of 1:1.8:35, stirring for 10 hours at the temperature of 30 ℃ to obtain hydrophilic silica-soluble collagen liquid, taking out 10ml of the silica-soluble collagen liquid, taking out 0.8ml of hexamethyldisilazane, uniformly mixing, then adding 0.2g of silicon dioxide nano powder particles, uniformly stirring at the normal temperature to obtain suspension, taking out 700 mu L suspension, mixing with 1m L absolute ethyl alcohol, carrying out ultrasonic oscillation for 1 hour, and forming a film on the surfaces of different base materials by using a pulling method.
The contact angle, roughness and transmittance of the coating surface prepared by the above method were measured, and the results are shown in fig. 4. As can be seen from the figure, the coating contact angle is 165.1 degrees, and is in a super-hydrophobic state; the transmittance data of the coated glass and the blank glass at 300-800nm are shown in FIG. 4, and the transmittance of the coated glass is very close to that of the blank glass, so that the coating obtained by the method is a transparent super-hydrophobic coating. The root mean square roughness of the coating surface is 348.6nm through surface roughness test.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (10)
1. A preparation method of a transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness is characterized by comprising the following steps:
(1) taking tetraethoxysilane, ammonia water and absolute ethyl alcohol as raw materials, mixing and stirring to prepare hydrophilic silica-soluble collagen liquid;
(2) uniformly mixing silicon-soluble collagen liquid and a siloxane reagent or a fluorosilane reagent, then adding silicon dioxide nano powder particles into the mixture, and uniformly stirring the mixture at normal temperature to obtain suspension;
(3) and (3) mixing the suspension with absolute ethyl alcohol, performing ultrasonic oscillation, and coating the mixture on the surface of a base material to form a film, thus obtaining the transparent super-coating, wherein the transparent super-coating has different hydrophilicity and hydrophobicity and different surface roughness according to different parameters of the steps (1) - (3).
2. The method for preparing the transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness according to claim 1, wherein the method comprises the following steps: in the step (1), the volume ratio of the ethyl orthosilicate to the ammonia water to the absolute ethyl alcohol is 1:1: 35-1: 3:35, and the stirring temperature is 30-60 ℃.
3. The method for preparing the transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness according to claim 1, wherein the method comprises the following steps: the silica-soluble collagen solution obtained in the reaction in the step (1) is light blue solution in which 20-50nm of silicon dioxide is uniformly dispersed.
4. The method for preparing the transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness according to claim 1, wherein the method comprises the following steps: the siloxane or fluorosilane reagent in the reaction in the step (2) is any one of methyltriethoxysilane, methyltrichlorosilane, hexamethyldisilazane, trimethylchlorosilane, perfluorodecyltrimethoxysilane, tridecafluorooctyltrimethoxysilane and the like.
5. The method for preparing the transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness according to claim 1, wherein the method comprises the following steps: and (3) adding the silicon dioxide nano powder into the reaction in the step (2) with the size of 7-60 nm.
6. The method for preparing the transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness according to claim 1, wherein the method comprises the following steps: the amount of the silicon dioxide nanopowder added in the reaction of the step (2) is 0.02g of the silicon dioxide nanopowder in 1ml of the silica-soluble collagen solution.
7. The method for preparing the transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness according to claim 1, wherein the method comprises the following steps: the volume ratio of the silica-soluble collagen solution to the siloxane reagent in the reaction in the step (2) is 1: 0-1: 0.1, and the wettability of the prepared transparent coating gradually changes from super-hydrophilic to super-hydrophobic along with the sequential change of the ratio of the silica-soluble collagen solution to the siloxane reagent in the interval.
8. The method for preparing the transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness as claimed in claim 1, wherein the volume of the suspension taken out from the reaction of the step (3) is 75-800 μ L, and the suspension is mixed with 1m L of absolute ethyl alcohol, thereby preparing the transparent coating with the root mean square roughness varying from tens of nanometers to hundreds of nanometers.
9. The method for preparing the transparent coating with adjustable hydrophilicity and hydrophobicity and surface roughness according to claim 1, wherein the method comprises the following steps: and (3) in the reaction of the step (3), the substrate is glass, plastic, a photovoltaic plate, a metal plate or a rubber plate, and the coating mode is a pulling method, a spin coating method or a spraying method.
10. A hydrophilic-hydrophobic transparent coating layer having adjustable surface roughness prepared by the preparation method as claimed in any one of claims 1 to 9.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111995889A (en) * | 2020-08-27 | 2020-11-27 | 马银屏 | Preparation method of sprayable hydrophobic material |
| CN112331037A (en) * | 2020-11-09 | 2021-02-05 | 济南大学 | System and method for visually displaying relationship between roughness and hydrophilicity and hydrophobicity |
| CN114479155A (en) * | 2022-03-03 | 2022-05-13 | 科伦塑业集团股份有限公司 | Super-hydrophilic antifogging nano film for agricultural film and preparation method thereof |
| CN115785813A (en) * | 2022-11-25 | 2023-03-14 | 东莞理工学院 | Super-hydrophilic porous coating with convertible transparency, preparation method and application thereof |
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| CN105599077A (en) * | 2015-12-18 | 2016-05-25 | 中国林业科学研究院木材工业研究所 | Method for preparation of superhydrophobic timber on the basis of sol-gel method |
| CN105949499A (en) * | 2016-07-11 | 2016-09-21 | 四川大学 | Preparation method for super-hydrophobic material |
| CN106009791A (en) * | 2016-05-16 | 2016-10-12 | 东南大学 | Super-hydrophilic particle hybridized super-hydrophobic coating and preparation method thereof |
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| CN101880478A (en) * | 2010-06-17 | 2010-11-10 | 华南理工大学 | Method for preparing hydrophobic nano-silica with controllable grain diameter |
| CN105599077A (en) * | 2015-12-18 | 2016-05-25 | 中国林业科学研究院木材工业研究所 | Method for preparation of superhydrophobic timber on the basis of sol-gel method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111995889A (en) * | 2020-08-27 | 2020-11-27 | 马银屏 | Preparation method of sprayable hydrophobic material |
| CN112331037A (en) * | 2020-11-09 | 2021-02-05 | 济南大学 | System and method for visually displaying relationship between roughness and hydrophilicity and hydrophobicity |
| CN114479155A (en) * | 2022-03-03 | 2022-05-13 | 科伦塑业集团股份有限公司 | Super-hydrophilic antifogging nano film for agricultural film and preparation method thereof |
| CN115785813A (en) * | 2022-11-25 | 2023-03-14 | 东莞理工学院 | Super-hydrophilic porous coating with convertible transparency, preparation method and application thereof |
| CN115785813B (en) * | 2022-11-25 | 2023-08-15 | 东莞理工学院 | Super-hydrophilic porous coating with changeable transparency, preparation method and application thereof |
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Application publication date: 20200731 |