CN114082617A - Hydrophobic coating with strong adhesion to substrate and preparation method thereof - Google Patents
Hydrophobic coating with strong adhesion to substrate and preparation method thereof Download PDFInfo
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- CN114082617A CN114082617A CN202111277152.2A CN202111277152A CN114082617A CN 114082617 A CN114082617 A CN 114082617A CN 202111277152 A CN202111277152 A CN 202111277152A CN 114082617 A CN114082617 A CN 114082617A
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- 239000000758 substrate Substances 0.000 title claims abstract description 90
- 238000000576 coating method Methods 0.000 title claims abstract description 61
- 239000011248 coating agent Substances 0.000 title claims abstract description 60
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 53
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002086 nanomaterial Substances 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- AVXLXFZNRNUCRP-UHFFFAOYSA-N trichloro(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctyl)silane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)[Si](Cl)(Cl)Cl AVXLXFZNRNUCRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 3
- 238000005507 spraying Methods 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005543 nano-size silicon particle Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 3
- 239000005751 Copper oxide Substances 0.000 claims description 3
- 229910000431 copper oxide Inorganic materials 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 239000010980 sapphire Substances 0.000 claims description 3
- 238000004528 spin coating Methods 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 238000005229 chemical vapour deposition Methods 0.000 claims description 2
- 238000001548 drop coating Methods 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 239000011247 coating layer Substances 0.000 claims 1
- 230000003075 superhydrophobic effect Effects 0.000 abstract description 28
- 239000000853 adhesive Substances 0.000 abstract description 12
- 230000001070 adhesive effect Effects 0.000 abstract description 12
- 239000012790 adhesive layer Substances 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 description 11
- 238000002844 melting Methods 0.000 description 9
- 230000008018 melting Effects 0.000 description 9
- 238000012360 testing method Methods 0.000 description 6
- 238000000137 annealing Methods 0.000 description 5
- 238000007664 blowing Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 230000003068 static effect Effects 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- -1 polydimethylsiloxane Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- ALVYUZIFSCKIFP-UHFFFAOYSA-N triethoxy(2-methylpropyl)silane Chemical compound CCO[Si](CC(C)C)(OCC)OCC ALVYUZIFSCKIFP-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
- B05D3/0272—After-treatment with ovens
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0493—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases using vacuum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
- B05D3/107—Post-treatment of applied coatings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/14—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by electrical means
- B05D3/141—Plasma treatment
- B05D3/145—After-treatment
-
- 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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2401/00—Form of the coating product, e.g. solution, water dispersion, powders or the like
- B05D2401/10—Organic solvent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2430/00—Component used as a filler in the composition
Abstract
The invention provides a hydrophobic coating with strong adhesive force with a substrate and a preparation method thereof, wherein the preparation method sequentially comprises the following steps: dispersing the nano material in an ethanol solution, then performing ultrasonic dispersion for 10-30min, and then coating the nano material on a substrate material; putting the sprayed substrate material into a vacuum muffle furnace, heating to 500-700 ℃ at the heating rate of 3 ℃/min, keeping for 3-5h, taking out and cooling to room temperature; and (3) treating the annealed substrate material for 8-12min by using oxygen plasma, then placing the annealed substrate material and perfluorooctyl trichlorosilane in a vacuum atmosphere, and fluorinating for 1-3h at room temperature to obtain the hydrophobic coating with strong adhesive force with the substrate. The invention also comprises the super-hydrophobic coating prepared by the method. The preparation method disclosed by the invention is simple and convenient, strong in controllability and lower in preparation cost, and effectively solves the problems that the super-hydrophobic coating primer adhesive layer is easy to age and decompose, easy to fall off, poor in stability and the like in the prior art.
Description
Technical Field
The invention belongs to the technical field of super-hydrophobic coating preparation, and particularly relates to a hydrophobic coating with strong adhesion to a substrate and a preparation method thereof.
Background
The super-hydrophobic material is a special material with a static contact angle of more than 150 degrees and a rolling angle of less than 10 degrees on the surface of the material. Because water drops have extremely high movement capacity on the surface of the material, the super-hydrophobic material is widely applied to the fields of self-cleaning, pollution prevention, water collection, mass and heat transfer enhancement, anti-icing, pipeline drag reduction and the like. The super-hydrophobic material can be obtained by preparing micro-nano roughness on the surface of a substrate and then carrying out surface energy reduction treatment on the micro-nano roughness; the superhydrophobic coating can also be obtained by attaching nanoparticles of a low surface energy material to a substrate by spraying, spin coating, pulling, self-assembly, and the like. However, the micro-nano structure is very fragile, the preparation process is complex and expensive, and the micro-nano structure cannot withstand strong friction; the super-hydrophobic coating greatly simplifies the preparation process and reduces the cost for manufacturing the super-hydrophobic material. Generally, a super-hydrophobic coating needs to use a polymer primer to enhance adhesion between the micro-nano structure and the substrate, and commonly used primer layers include acrylate, polydimethylsiloxane, isobutyl triethoxysilane, and the like. However, in practical application, the primer bonding layer is easy to age and even decompose under the influence of factors such as high temperature, ultraviolet irradiation, salt spray corrosion and the like. Finally, the super-hydrophobic coating is peeled off, and the scale development of the super-hydrophobic coating is severely limited by the problem. Therefore, it is necessary to develop a method for enhancing the adhesion between the super-hydrophobic coating and the substrate without a high-molecular primer adhesive layer.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the hydrophobic coating with strong adhesive force with the substrate and the preparation method thereof, the preparation method is simple and convenient, the controllability is strong, the preparation cost is lower, and the problems that the primer adhesive layer of the super-hydrophobic coating in the prior art is easy to age and decompose, easy to fall off, poor in stability and the like are effectively solved.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the hydrophobic coating with strong adhesive force with the substrate comprises the following steps in sequence:
(1) dispersing the nano material in an ethanol solution with the concentration of 90-98 vt%, then carrying out ultrasonic dispersion for 10-30min under the power of 300-500W, and then coating the nano material on a substrate material;
(2) putting the sprayed substrate material into a vacuum muffle furnace, heating to 500-700 ℃ at the heating rate of 3 ℃/min, keeping for 3-5h, taking out and cooling to room temperature;
(3) and (3) treating the annealed substrate material by using oxygen plasma for 8-12min, then placing the substrate material and 100-200 mu L of perfluorooctyl trichlorosilane in a vacuum atmosphere, and fluorinating the substrate material for 1-3h at room temperature to obtain the hydrophobic coating with strong adhesion to the substrate.
Furthermore, the mass-volume ratio of the nano material to the ethanol solution is 0.4-0.6:20 g/mL.
Further, the mass-volume ratio of the nano material to the ethanol solution is 0.5:20 g/mL.
Further, the nano material is nano silicon dioxide, titanium dioxide, zinc oxide or copper oxide.
Further, in the step (1), the coating mode is chemical vapor deposition, spray coating, pulling, spin coating or drop coating.
Further, the coating is sprayed on the base material under a pressure of 0.2-0.4MPa, with a spraying distance of 10 cm.
Further, the substrate material is glass, alumina or sapphire.
Further, in the step (2), after being taken out, the substrate material is blown to two sides by high-pressure cold air and is uniformly cooled to room temperature.
The hydrophobic coating with strong adhesive force with the substrate is prepared by the preparation method of the hydrophobic coating with strong adhesive force with the substrate.
In summary, the invention has the following advantages:
1. the preparation method disclosed by the invention is simple and convenient, strong in controllability and lower in preparation cost, and effectively solves the problems that the super-hydrophobic coating primer adhesive layer is easy to age and decompose, easy to fall off, poor in stability and the like in the prior art.
2. The invention attaches the nano material on the surface of the substrate material, the surface can be a flat surface without structure, and a microstructure can also be manufactured on the flat surface, the microstructure comprises a columnar structure, a conical structure, an inverted pyramid structure, an inverted triangular pyramid structure and an inverted hexagonal pyramid structure, then the high-temperature annealing is carried out to reach the softening temperature of the substrate and the nano material, the high-strength adhesion of the nano material and the substrate can be realized without a high-molecular adhesive, and finally the surface energy of the substrate layer is reduced through fluorination to obtain the super-hydrophobic coating. The method is simple and convenient, strong in controllability and low in cost, the prepared super-hydrophobic coating has strong mechanical stability, is resistant to acid and alkali corrosion, is high in optical transmittance, keeps long-acting super-hydrophobicity in a humid environment, has wide application prospect, and is expected to realize industrialization.
3. And the softening temperature of the nano particles is reached in the annealing process, the melting coupling of the nano particles is realized, and meanwhile, the partial mutual melting of the nano particles close to the substrate and the substrate is realized, so that the nano particles and the substrate are coupled, and the stability of the coating is enhanced. During the annealing process, the annealing temperature should be controlled, and different nano materials and substrates should be selected to have proper temperatures to prevent the whole melting of the nano particles and the whole melting of the substrates, so that the annealing temperature should be kept below the melting temperature of the nano particles, and the melting temperature of the selected substrate material should be lower than the melting temperature of the nano particles.
4. According to the invention, the nano particles are softened at high temperature and are directly and tightly connected with the substrate layer, so that the problems of non-durability and non-wear resistance of the super-hydrophobic coating are solved, the adhesive tape can be repeatedly torn and pulled for 500 times, and the friction and wear test lasts for 1h, so that the good super-hydrophobic performance can be still maintained, and the practical application of the super-hydrophobic coating is realized.
Drawings
FIG. 1 is a schematic diagram showing comparison before and after calcination and melting;
FIG. 2 is an SEM image of the surface morphology of calcined nano-silica;
FIG. 3 is a static contact angle of a surface after a frictional wear test;
FIG. 4 is a dynamic contact angle of a surface after frictional wear.
Detailed Description
Example 1
The preparation method of the hydrophobic coating with strong adhesion to a substrate sequentially comprises the following steps:
(1) dispersing 0.5g of nano silicon dioxide in 20ml of ethanol solution with the concentration of 95vt percent, then ultrasonically dispersing for 20min under the power of 400W, and then spraying on a substrate material (glass sheet) under the pressure of 0.3 MPa;
(2) putting the sprayed substrate material into a vacuum muffle furnace, heating to 600 ℃ at the heating rate of 3 ℃/min, keeping for 4h, taking out, blowing high-pressure cold air to two sides of the substrate material, and uniformly cooling to room temperature;
(3) and (3) treating the annealed substrate material for 10min by using oxygen plasma, then placing the substrate material and 100 mu L of perfluorooctyl trichlorosilane in a vacuum atmosphere, and fluorinating for 2h at room temperature to obtain the hydrophobic coating with strong adhesive force with the substrate.
Example 2
The preparation method of the hydrophobic coating with strong adhesion to a substrate sequentially comprises the following steps:
(1) dispersing 0.5g of nano titanium dioxide in 20ml of ethanol solution with the concentration of 95vt percent, then ultrasonically dispersing for 20min under the power of 400W, and then spraying on a substrate material (glass sheet) under the pressure of 0.3MPa, wherein the spraying distance is 10 cm;
(2) putting the sprayed substrate material into a vacuum muffle furnace, heating to 600 ℃ at the heating rate of 3 ℃/min, keeping for 4h, taking out, blowing high-pressure cold air to two sides of the substrate material, and uniformly cooling to room temperature;
(3) and (3) treating the annealed substrate material for 10min by using oxygen plasma, then placing the substrate material and 100 mu L of perfluorooctyl trichlorosilane in a vacuum atmosphere, and fluorinating for 2h at room temperature to obtain the hydrophobic coating with strong adhesive force with the substrate.
Example 3
The preparation method of the hydrophobic coating with strong adhesion to a substrate sequentially comprises the following steps:
(1) dispersing 0.5g of nano zinc oxide in 20ml of ethanol solution with the concentration of 95vt percent, then ultrasonically dispersing for 20min under the power of 400W, and then spraying on a glass sheet with an inverted pyramid structure under the pressure of 0.3MPa, wherein the spraying distance is 10 cm;
(2) putting the sprayed substrate material into a vacuum muffle furnace, heating to 600 ℃ at the heating rate of 3 ℃/min, keeping for 4h, taking out, blowing high-pressure cold air to two sides of the substrate material, and uniformly cooling to room temperature;
(3) and (3) treating the annealed substrate material for 10min by using oxygen plasma, then placing the substrate material and 100 mu L of perfluorooctyl trichlorosilane in a vacuum atmosphere, and fluorinating for 2h at room temperature to obtain the hydrophobic coating with strong adhesive force with the substrate.
Example 4
The preparation method of the hydrophobic coating with strong adhesion to a substrate sequentially comprises the following steps:
(1) dispersing 0.5g of nano copper oxide in 20ml of ethanol solution with the concentration of 95vt percent, then ultrasonically dispersing for 20min under the power of 400W, and then spraying on a substrate material (aluminum oxide) under the pressure of 0.3MPa, wherein the spraying distance is 10 cm;
(2) putting the sprayed substrate material into a vacuum muffle furnace, heating to 600 ℃ at the heating rate of 3 ℃/min, keeping for 4h, taking out, blowing high-pressure cold air to two sides of the substrate material, and uniformly cooling to room temperature;
(3) and (3) treating the annealed substrate material for 10min by using oxygen plasma, then placing the substrate material and 100 mu L of perfluorooctyl trichlorosilane in a vacuum atmosphere, and fluorinating for 2h at room temperature to obtain the hydrophobic coating with strong adhesive force with the substrate.
Example 5
The preparation method of the hydrophobic coating with strong adhesion to a substrate sequentially comprises the following steps:
(1) dispersing 0.5g of nano silicon dioxide in 20ml of ethanol solution with the concentration of 95vt percent, then ultrasonically dispersing for 20min under the power of 400W, and then spraying on a substrate material (sapphire) under the pressure of 0.3MPa, wherein the spraying distance is 10 cm;
(2) putting the sprayed substrate material into a vacuum muffle furnace, heating to 600 ℃ at the heating rate of 3 ℃/min, keeping for 4h, taking out, blowing high-pressure cold air to two sides of the substrate material, and uniformly cooling to room temperature;
(3) and (3) treating the annealed substrate material for 10min by using oxygen plasma, then placing the substrate material and 100 mu L of perfluorooctyl trichlorosilane in a vacuum atmosphere, and fluorinating for 2h at room temperature to obtain the hydrophobic coating with strong adhesive force with the substrate.
The superhydrophobic coatings obtained from examples 1-5 were subjected to performance testing, the superhydrophobicity was performed according to the standard tear test, and the results are shown in table 1.
Table 1 performance test data
As can be seen from Table 1, through multiple coating peeling test experiments, the super-hydrophobic coating obtained by the invention still has super-hydrophobic performance and very strong mechanical stability, and effectively solves the problems that the primer bonding layer of the super-hydrophobic coating in the prior art is easy to age, decompose and peel.
A schematic comparison diagram of the super-hydrophobic coating obtained in example 1 before and after calcination and melting, an SEM image of the surface morphology of the calcined nano-silica, a static contact angle of the surface after a frictional wear test, and a dynamic contact angle of the surface after frictional wear are respectively obtained, as shown in fig. 1 to 4.
As can be seen from fig. 1, fusion occurs between the nanoparticles and the substrate, coupling the nanoparticles and the substrate, thereby enhancing the stability of the coating. As can be seen from FIG. 2, the superhydrophobic coating surface was formed uniformly. As can be seen from fig. 3 and 4, the super-hydrophobic coating after frictional wear still has super-hydrophobic properties, has better stability, and is not easy to fall off.
While the present invention has been described in detail with reference to the illustrated embodiments, it should not be construed as limited to the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (9)
1. The preparation method of the hydrophobic coating with strong adhesion to the substrate is characterized by sequentially comprising the following steps of:
(1) dispersing the nano material in an ethanol solution with the concentration of 90-98 vt%, then carrying out ultrasonic dispersion for 10-30min under the power of 300-500W, and then coating the nano material on a substrate material;
(2) putting the sprayed substrate material into a vacuum muffle furnace, heating to 500-700 ℃ at the heating rate of 3 ℃/min, keeping for 3-5h, taking out and cooling to room temperature;
(3) and (3) treating the annealed substrate material by using oxygen plasma for 8-12min, then placing the substrate material and 100-200 mu L of perfluorooctyl trichlorosilane in a vacuum atmosphere, and fluorinating the substrate material for 1-3h at room temperature to obtain the hydrophobic coating with strong adhesion to the substrate.
2. The method for preparing the hydrophobic coating with strong adhesion to the substrate according to claim 1, wherein the mass-to-volume ratio of the nano material to the ethanol solution is 0.4-0.6:20 g/mL.
3. The method for preparing the hydrophobic coating with strong adhesion to the substrate according to claim 2, wherein the mass-to-volume ratio of the nano material to the ethanol solution is 0.5:20 g/mL.
4. The method for preparing the hydrophobic coating with strong adhesion to the substrate according to claim 1, wherein the nano material is nano silicon dioxide, titanium dioxide, zinc oxide or copper oxide.
5. The method for preparing the hydrophobic coating layer with strong adhesion to the substrate according to claim 1, wherein in the step (1), the coating manner is chemical vapor deposition, spray coating, lifting, spin coating or drop coating.
6. The method for preparing a hydrophobic coating with strong adhesion to a substrate according to claim 1, wherein the coating is sprayed on the substrate material at a distance of 10cm under a pressure of 0.2 to 0.4 MPa.
7. The method of claim 1, wherein the substrate is made of glass, alumina or sapphire.
8. The method for preparing a hydrophobic coating with strong adhesion to a substrate according to claim 1, wherein in the step (2), the coating is taken out and blown to both sides of the substrate material by high-pressure cold air, and is uniformly cooled to room temperature.
9. The hydrophobic coating with strong adhesion to the substrate prepared by the method for preparing the hydrophobic coating with strong adhesion to the substrate as claimed in any one of claims 1 to 8.
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