CN108033688B - Silicon oxide-based super-hydrophobic coating and preparation method thereof - Google Patents
Silicon oxide-based super-hydrophobic coating and preparation method thereof Download PDFInfo
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/001—General methods for coating; Devices therefor
- C03C17/002—General methods for coating; Devices therefor for flat glass, e.g. float glass
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/44—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the composition of the continuous phase
- C03C2217/45—Inorganic continuous phases
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
- C03C2217/475—Inorganic materials
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/112—Deposition methods from solutions or suspensions by spraying
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/17—Deposition methods from a solid phase
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/31—Pre-treatment
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Abstract
The invention relates to a silicon oxide-based super-hydrophobic coating and a preparation method thereof, wherein the silicon oxide-based super-hydrophobic coating comprises a substrate and is characterized in that the substrate is coated with a spherical quartz powder A, a bottom film layer prepared from ethanol, a middle film layer prepared from spherical quartz powder, tetraethoxysilane, ethanol and dilute hydrochloric acid, and a surface film layer prepared from fluorosilane solution by spraying. a. Dispersing spherical quartz powder A in ethanol to form suspension; b. cleaning the glass sheet, soaking the glass sheet in a mixed solution of concentrated sulfuric acid and hydrogen peroxide, and drying to obtain a glass substrate; c. immersing the glass substrate into the suspension, taking out and drying to obtain a quartz foundation film layer; d. mixing tetraethoxysilane and ethanol, stirring, and adding dilute hydrochloric acid to prepare silicon dioxide sol; e. adding spherical quartz powder B into the silica sol, and mixing to obtain a mixed solution; f. coating the mixed solution on the quartz foundation film layer, drying and sintering to obtain an intermediate film layer; g. and spraying fluorosilane solution on the surface of the intermediate film layer, and curing. The silicon oxide-based super-hydrophobic coating has the advantages of firmness, durability and good chemical stability, can be used on the surfaces of materials such as ceramics, glass and the like, and has the characteristics of pollution prevention, fingerprint prevention, oxidation prevention, hydrophobicity and the like.
Description
Technical Field
The invention belongs to the technical field of hydrophobic coatings, relates to a silicon oxide-based super-hydrophobic coating and also relates to a preparation method of the silicon oxide-based super-hydrophobic coating.
Background
The superhydrophobic surface has a water contact angle greater than 150 ° and a low roll off angle (less than 10 °). The method for realizing the super-hydrophobicity comprises the following steps: vertical array nanotubes and nanofibers, sol-gel method (sol-gel), phase separation method, layer-by-layer self-assembly (LBL), grazing angle deposition, and the like. Among these techniques, the sol-gel method is simpler and more efficient than other methods in the technique of depositing a superhydrophobic coating, and at the same time, it has significant advantages in that it can coat a large area, the surface shape of the deposited object is not limited, and the coating time is short. Two major factors affecting the wettability of a solid surface are the surface chemical composition (surface free energy) and the surface topography (roughness), respectively. Superhydrophobicity is the result of a combination of specific roughness structures and low surface energy materials. To achieve superhydrophobicity, a rough surface may be obtained first, followed by a low surface energy, or a rough structure with low surface energy may be achieved at the same time.
The contact area of solid and liquid is reduced due to the rough structure of the super-hydrophobic surface, and meanwhile, the contact area of the surface and pollutants is small, so that the acting force between the surface and the pollutants is weakened; when the liquid drops roll, the pollutants on the super-hydrophobic surface are easily taken away, and the unique self-cleaning property enables the super-hydrophobic liquid drops to have wide application prospects in industrial and agricultural production, national defense construction and daily life.
Disclosure of Invention
The invention aims to produce a coating with self-cleaning property, and provides a silicon oxide-based super-hydrophobic coating and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a silicon oxide-based super-hydrophobic coating comprises a substrate, and is characterized in that the substrate is sequentially coated with a bottom film layer prepared from spherical quartz powder A and ethanol, an intermediate film layer prepared from spherical quartz powder B, tetraethoxysilane, ethanol and dilute hydrochloric acid, and a surface film layer prepared by spraying a fluorosilane solution; wherein, the base film layer comprises the following raw materials: the mass concentration of the absolute ethyl alcohol mixed solution is 8% -13% of spherical quartz powder A with the particle size of 0.8-4 mu m, and the mixture ratio of the raw materials of the middle film layer is as follows: according to the mass parts, spherical quartz powder B2-4 with the granularity of 0.1-0.8 mu m, tetraethoxysilane 15-20, absolute ethyl alcohol 28-33 and dilute hydrochloric acid 10-14.
A preparation method of a silicon oxide-based super-hydrophobic coating is characterized by comprising the following steps:
a. weighing the raw materials according to the mass part ratio, dispersing spherical quartz powder A with the granularity of 0.8-4 mu m (preferably 2-4 mu m) in absolute ethyl alcohol, controlling the mass concentration of absolute ethyl alcohol mixed liquor of the quartz powder A to be 8-13%, fully stirring, and carrying out ultrasonic oscillation to form uniform suspension;
b. sequentially ultrasonically cleaning a glass sheet by absolute ethyl alcohol and deionized water, then putting a mixed solution consisting of concentrated sulfuric acid with the concentration of 98% and hydrogen peroxide with the concentration of 30% according to the volume ratio of 3:1, soaking for 1h at the temperature of 80 ℃, and drying to obtain an activated and fresh glass substrate;
c. b, immersing the glass substrate obtained in the step b into the suspension obtained in the step a, standing for 20s, taking out, drying for 15-30 min at 100 ℃ in a drying oven, then placing in a muffle furnace at 580-600 ℃ to soften the surface of the glass, embedding the quartz powder at the bottommost layer into the surface of the glass under the action of gravity and bonding together, preserving heat for 30min, taking out, washing with deionized water, and obtaining a quartz foundation film layer on the glass;
d. weighing 15-20 parts of tetraethoxysilane and 28-33 parts of absolute ethyl alcohol according to the mass part ratio, mixing, hydrolyzing, magnetically stirring for 1 hour, and then adding 10-14 parts of dilute hydrochloric acid of 0.1mol/L for condensation reaction for 4 hours to prepare silicon dioxide sol;
e. adding spherical quartz powder B with the particle size of 0.1-0.8 mu m (preferably 0.1-0.4 mu m) into the silicon dioxide sol, controlling the ultrasonic power to be 300W and the frequency to be 40KHz, and oscillating and dispersing for 30min to obtain a mixed solution of the silicon dioxide sol and the quartz powder B;
f. coating the mixed solution prepared in the step e on the quartz foundation film layer obtained in the step c, drying at 120 ℃ for 30-60 min, and sintering at 350-420 ℃ for 20-30 min to obtain an intermediate film layer of the super-hydrophobic film;
g. and f, spraying a fluorosilane solution on the surface of the intermediate film layer obtained in the step f by using a spray gun, and curing at the temperature of 100-150 ℃ for 60-120 min to obtain the silicon oxide-based super-hydrophobic coating.
Further, a preparation method of the silicon oxide-based super-hydrophobic coating comprises the following steps: adding 49mL of ethylene glycol pure solvent into 50mL of deionized water, slowly adding 1 mL of heptadecafluorodecyltrimethoxysilane, uniformly stirring by magnetic force, adding oxalic acid to control the pH value to be about 3.0, stirring for 1h, and standing for 5h to fully hydrolyze to obtain the heptadecafluorodecyltrimethoxysilane.
In order to realize certain roughness and lower surface energy on the surface, the coating disclosed by the invention is composed of three layers, namely a spherical quartz powder bottom layer, a silica sol middle layer and a fluorosilane surface layer.
The invention has the beneficial effects that the silicon oxide-based super-hydrophobic coating is firm and durable and has good chemical stability; can be applied to the surfaces of materials such as ceramics, glass and the like, and has the excellent properties of pollution prevention, fingerprint prevention, oxidation prevention, hydrophobicity and the like.
Detailed Description
A silicon oxide-based super-hydrophobic coating and a preparation method thereof are disclosed, and the specific implementation steps are as follows:
example 1
(1) Dispersing 10g of spherical quartz powder A with the particle size of 2-4 microns in 100 mL of absolute ethyl alcohol, fully stirring, putting into an ultrasonic cleaning machine, heating in a water bath to 50 ℃, and oscillating for 30min at the ultrasonic power of 300W and the frequency of 40KHz to form uniform suspension;
(2) sequentially ultrasonically cleaning a 76mm by 25mm by 1mm glass sheet for 15min by using absolute ethyl alcohol and deionized water, then putting a mixed solution consisting of concentrated sulfuric acid with the concentration of 98% and hydrogen peroxide with the concentration of 30% in a volume ratio of 3:1, soaking for 1h at the temperature of 80 ℃, and drying to obtain an activated and fresh glass substrate;
(3) horizontally immersing the glass substrate obtained in the step (2) into the suspension obtained in the step (1), standing for 20s, horizontally taking out, drying for 10min in a drying oven at the temperature of 100 ℃, then placing in a muffle furnace at the temperature of 580 ℃ for heat preservation for 30min, taking out a sample, washing with deionized water to remove redundant quartz powder which is not firmly combined, and forming a quartz foundation film layer with a single particle layer on the surface of glass;
(4) mixing 41.8 mL of absolute ethyl alcohol with 20mL of tetraethoxysilane, magnetically stirring for 1h at room temperature, then dripping 13 mL of 0.1mol/L hydrochloric acid solution, and stirring for 4h to obtain colorless transparent silica sol;
(5) adding 2.98g of spherical quartz powder B with the particle size of 0.1-0.4 mu m into the silicon dioxide sol, oscillating and dispersing for 30min at the ultrasonic power of 300W and the frequency of 40KHz, and preparing a gel film from the quartz foundation film layer prepared in the step (3) by adopting a dipping and pulling method, wherein the pulling rate is 130mm/min, and the dipping time is 40s, so as to obtain an intermediate film layer;
(6) adding 49mL of ethylene glycol pure solvent into 50mL of deionized water, slowly adding 1 mL of heptadecafluorodecyltrimethoxysilane, uniformly stirring by magnetic force, adding oxalic acid to control the pH value to be about 3.0, stirring for 1h to uniformly disperse fluorosilane, standing for 5h to fully hydrolyze fluorosilane to obtain fluorosilane solution, putting the prepared fluorosilane solution into a paint storage tank of compressed air spraying and coating equipment, wherein the caliber of a paint nozzle is 0.8mm, the paint air pressure is 0.29MPa, the air flow is 270L/min, the paint spraying amount is 150mL/min, the distance between the nozzle and the surface of an intermediate membrane layer is 20cm, uniformly spraying for 5s to form a top fluorosilane membrane layer, draining off the excess fluorosilane solution at room temperature, placing the top fluorosilane membrane layer in a drying oven, and drying for 1.5h at 120 ℃ to obtain the silicon oxide-based.
Claims (2)
1. A preparation method of a silicon oxide-based super-hydrophobic coating is characterized by comprising the following steps:
a. weighing raw materials according to the mass part ratio, dispersing spherical quartz powder A with the granularity of 0.8-4 mu m in absolute ethyl alcohol, controlling the mass concentration of the quartz powder A in the dispersant absolute ethyl alcohol to be 8-13%, fully stirring, and performing ultrasonic oscillation to form uniform suspension;
b. sequentially ultrasonically cleaning a glass sheet by absolute ethyl alcohol and deionized water, then putting a mixed solution consisting of concentrated sulfuric acid with the concentration of 98% and hydrogen peroxide with the concentration of 30% according to the volume ratio of 3:1, soaking for 1h at the temperature of 80 ℃, and drying to obtain an activated and fresh glass substrate;
c. b, immersing the glass substrate obtained in the step b into the suspension obtained in the step a, standing for 20s, taking out, drying in a drying oven at 100 ℃ for 15-30 min, then placing in a muffle furnace at 580-600 ℃ for heat preservation for 30min, taking out, washing with deionized water, and obtaining a quartz foundation film layer on the glass;
d. weighing 15-20 parts of tetraethoxysilane and 28-33 parts of absolute ethyl alcohol according to the mass part ratio, mixing, hydrolyzing, magnetically stirring for 1 hour, and then adding 10-14 parts of dilute hydrochloric acid of 0.1mol/L for condensation reaction for 4 hours to prepare silicon dioxide sol;
e. adding 2-4 parts of spherical quartz powder B with the granularity of 0.1-0.8 mu m into the silicon dioxide sol, controlling the ultrasonic power to be 300W and the frequency to be 40KHz, and oscillating and dispersing for 30min to obtain a mixed solution of the silicon dioxide sol and the quartz powder B;
f. coating the mixed solution prepared in the step e on the quartz foundation film obtained in the step c, drying at 120 ℃ for 30-60 min, and sintering at 350-420 ℃ for 20-30 min to obtain an intermediate film layer of the super-hydrophobic film;
g. and f, spraying a fluorosilane solution on the surface of the intermediate film layer obtained in the step f by using a spray gun, and curing at the temperature of 100-150 ℃ for 60-120 min to obtain the silicon oxide-based super-hydrophobic coating.
2. The preparation method of the silicon oxide-based super-hydrophobic coating according to claim 1, characterized in that the preparation method of the fluorosilane solution comprises the following steps: adding 49mL of ethylene glycol pure solvent into 50mL of deionized water, slowly adding 1 mL of heptadecafluorodecyltrimethoxysilane, uniformly stirring by magnetic force, adding oxalic acid to control the pH value to be about 3.0, stirring for 1h, and standing for 5h to fully hydrolyze to obtain the heptadecafluorodecyltrimethoxysilane.
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CN108977030B (en) * | 2018-07-26 | 2020-08-14 | 大连理工大学 | Preparation method of fluorinated halloysite nanotube/waterborne polyurethane composite hydrophobic coating |
CN110240420A (en) * | 2019-06-27 | 2019-09-17 | 广东星星精密玻璃科技有限公司 | A kind of long-acting anti-fingerprint film plated film spraying process of glass |
CN111420857B (en) * | 2019-09-12 | 2022-02-18 | 浙江海洋大学 | Preparation method of multilayer nano-porous marine antifouling coating |
CN116119674A (en) * | 2022-11-23 | 2023-05-16 | 安徽凯盛基础材料科技有限公司 | Method for preparing silicon dioxide hollow microspheres by hard template method |
CN117720277B (en) * | 2023-12-05 | 2024-06-14 | 江苏悦丰晶瓷科技有限公司 | Color glass ceramics and preparation method thereof |
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CN101234854A (en) * | 2006-02-01 | 2008-08-06 | 旭硝子株式会社 | Infrared shielding film-coated glass plate and production process therefor |
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CN1872661A (en) * | 2006-04-29 | 2006-12-06 | 东南大学 | Ultra hydrophobic surface material with multilevel structure, and preparation method |
CN103524053B (en) * | 2012-07-03 | 2015-05-27 | 中国科学院兰州化学物理研究所 | Preparation method of transparent super-hydrophobic coatings |
CN104802488B (en) * | 2014-01-27 | 2017-02-15 | 中国科学院过程工程研究所 | Super-hydrophobic coating layer used for oil-water separation and having hierarchical structure, super-hydrophobic material thereof, and preparation method of material |
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US5792327A (en) * | 1994-07-19 | 1998-08-11 | Corning Incorporated | Adhering metal to glass |
CN101234854A (en) * | 2006-02-01 | 2008-08-06 | 旭硝子株式会社 | Infrared shielding film-coated glass plate and production process therefor |
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