CN106517813B - The preparation method of the hydrophobic antifog glass of oleophobic and its coating - Google Patents
The preparation method of the hydrophobic antifog glass of oleophobic and its coating Download PDFInfo
- Publication number
- CN106517813B CN106517813B CN201610850662.7A CN201610850662A CN106517813B CN 106517813 B CN106517813 B CN 106517813B CN 201610850662 A CN201610850662 A CN 201610850662A CN 106517813 B CN106517813 B CN 106517813B
- Authority
- CN
- China
- Prior art keywords
- oleophobic
- glass
- hydrophobic
- coating
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
-
- 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
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
-
- 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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/76—Hydrophobic and oleophobic coatings
-
- 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
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/77—Coatings having a rough surface
-
- 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
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses the preparation methods of a kind of hydrophobic antifog glass of oleophobic and its coating, the preparation method of the hydrophobic antifog glass coating of the oleophobic, include the following steps: 1) to be activated glass sample, grafted fluoropolymer surfactant on the glass surface again, fluorine-containing coat is formed, makes glass surface that hydrophilic and oleophobic state be presented；2) plasma etching treatment is carried out to the glass sample surface by step 1) processing using sputtering plasma instrument and obtains the hydrophobic antifog glass coating of oleophobic, the effective power for sputtering plasma instrument is 400W~700W, discharge frequency is controlled in 13.56MHz frequency band, the flow for being passed through discharge gas is 0.4~0.8L/min, air pressure is 0.1~0.4 atmospheric pressure when electric discharge, and the processing time is 40~80min.The hydrophobic antifog glass surface energy of oleophobic obtained by above-mentioned processing is low, shows good hydrophobic oleophobic characteristic, anti-fog performance is good.
Description
Technical field
The present invention relates to a kind of antifog glass, the preparation side of a kind of hydrophobic antifog glass of oleophobic and its coating is particularly related to
Method.
Background technique
Glass plays a significant role in people's lives, but the atomizating phenomenon of glass surface is to the daily life of people
Living, work and production bring many inconvenience, in the modern life, according to the practical need of glass for building purposes and windshield etc.
It wants, in glass surface preparation there is waterproof, antifog, self-cleaning function hydrophobic, hydrophilic and its assembly of thin films just to have important
Meaning.For this purpose, a kind of developing direction and research hotspot at low cost, simple production process anti-fog coating is the field are developed,
Further this technology is developed on this basis to non-toxic, pollution-free direction simultaneously, and further develops and passes through chemical bond
It is also one of research hotspot that mode even, which prepares glass coating,.
From material surface wellability is changed, it is antifog antifog with hydrophily that the antifog technology of glass is divided into hydrophobicity.It is hydrophobic
Antifog property is to make substrate surface very hydrophobic, makes contact angle θ → 180 ° of material surface and water, tumbles the water droplet to be formed.
Antifog hydrophily is to make substrate surface highly-hydrophilized, makes contact angle θ → 0 ° of material surface and water, allows vapor in substrate table
Face is not easy to condense into droplet but forms transparent moisture film.
The anti-misting component of hydrophobicity anti-fog coating is fluorine-containing, silicon macromolecule resin.In terms of thin film-forming method, hydrophobicity is antifog
Coating can be divided mainly into physical absorption film and chemisorbed film two major classes.Physical absorption film mainly relies on van der Waals interaction handle
Grease, fluorocarbons substance (such as perfluorinated aliphatic acid and fatty alcohol), petroleum and its product (such as aphthenic acids) are adsorbed on base
The surface of material.Physical absorption film is in spite of good hydrophobic effect, but it is often intolerant to abrasion and not solvent-proof, and object
Reason adsorbed film can seriously affect the transparency of substrate coated on transparent substrate surface, thus this antifog technology is difficult to promote.Change
It learns adsorbed film and mainly passes through chemical bonds ruthenium trimethoxysilane, decyltrichlorosilane, ruthenium triethoxysilane, the last of the ten Heavenly stems
Base (methoxy ethoxy) silane, dimethyldimethoxysil,ne etc., these compounds can form permanent, firm in substrate surface
Solid transparent water film.
The antifog wetting property by improving substrate surface of hydrophily, reduces the contact angle of itself and water droplet, as contact angle θ
When tending to 0 °, vapor can be sprawled highly when substrate surface agglomerates, and form uniform moisture film, eliminate the diffusing reflection of light,
To reach anti-fog effect.Hydrophily anti-fog method mainly includes coating surface activating agent, inorganic sol coating, organic polymer
Hydrophily anti-fog coating, hybrid hydrophily anti-fog coating, photocatalysis ultra-hydrophilic surface and construct coarse structure or
Super hydrophilic antifogging surface of porous structure etc..
Chinese patent application, antireflective superhydrophilic self-cleaning SiO2Anti-fog coating and preparation method thereof, application number:
201010533381.1 disclosing a kind of antireflective superhydrophilic self-cleaning SiO2Anti-fog coating, anti-fog coating are to be by partial size
The shell of the outer surface of 49~100nm is thin and non-porous, mesoporous SiO of the hypostracum with mesoporous bivalve layer2Hollow sphere is in glass
The accumulation of glass surface is constituted, and the anti-fog coating surface has the coarse structure on nanoscale, thick on the nanoscale
Rough structure be made of accumulation the outer surface in the anti-fog coating shell be it is thin and non-porous, hypostracum is with mesoporous
The mesoporous SiO of bivalve layer2What the hole between hollow sphere particle within the scope of possessed nanoscale was formed；The outer surface
Shell be thin and non-porous, mesoporous SiO of the hypostracum with mesoporous bivalve layer2The structure of hollow sphere are as follows: diameter be 5~
It is with a thickness of 20~30nm outside the cavity of 30nm with mesoporous SiO2Mesoporous lamella has mesoporous SiO in described2It is situated between
The non-porous SiO that hole shell is coated with a thickness of 2~5nm2Shell.
Chinese patent application, suitable for the Ceramic precursor resin of glass rain-proof automatic cleaning coating, application number:
201110287424.7, the synthetic method of fluorine-containing poly- silicon nitrogen silicone resin is disclosed, and application is glass surface durability
The method of antirain agent coating.Fluorine-containing chlorosilane monomer mixture is formed into polysiloxane prepolymers by partial hydrolysis, is then passed through
It crosses and prepares fluorine-containing polysilazane-polysiloxane polymer with the amido exchange reaction of hexamethyldisilazane.Poly- silicon nitrogen siloxanes and glass
Surface is chemically bound together the protective film to form firm connection.The fluorinated polysiloxane bullet hydrolyzed to form in air
Property body coating hydrophobic, high-low temperature resistant and resistance to scribing, there is rain-proof, antifog and automatic cleaning action.
The anti-fog coating studied extensively at present, no matter hydrophilic coating or hydrophobic coating, only make glassy silicate
Glass has anti-fog effect, but the effect of water resistant oily pollution is little.
Summary of the invention
The purpose of the present invention is to provide the good hydrophobic antifog glass of oleophobic of a kind of simple process, water resistant oil effect and its paintings
The preparation method of layer.
To achieve the above object, the preparation method of the hydrophobic antifog glass coating of oleophobic provided by the present invention, including it is as follows
Step:
1) glass sample is activated, then grafted fluoropolymer surfactant on the glass surface, forms fluorine-containing painting
Layer makes glass surface that hydrophilic and oleophobic state be presented；
2) plasma etching treatment is carried out to the glass sample surface by step 1) processing using sputtering plasma instrument
The hydrophobic antifog glass coating of oleophobic is obtained, the effective power of sputtering plasma instrument is 400W~700W, and discharge frequency control exists
13.56MHz frequency band, the flow for being passed through discharge gas is 0.4~0.8L/min, and air pressure is absolute pressure 0.1~0.4 big when electric discharge
Air pressure (in this patent, unless otherwise indicated, electric discharge air pressure is absolute pressure), the processing time is 40~80min.Sputtering etc. from
The plasma that sub- instrument generates is low temperature plasma.
Mechanism of action: present invention grafted fluoropolymer surfactant first on the glass surface being activated is changed
It learns key to connect, forms fluoropolymer brush, so that hydrophilic and oleophobic state is presented in glass surface, then preparation is had into fluorine-containing coat table
The glass sample in face carries out corona treatment will form on the surface of the material due to the corrasion of ion collision material surface
Fine concave-convex sputters the substance diffusion into the surface in the plasma of generation, reassembles on the top of convex, as a result formed
A large amount of protrusions, material surface pattern change.
Optionally, in step 1), the specific steps of activation processing are as follows: 1.1) glass sample is immersed in hydrogen peroxide and dense sulphur
Heat in the mixing washing lotion of acid, until stopping heating when bubble-free generates；1.2) it takes out glass sample to be cooled to room temperature, be put into
Supersound washing in deionized water is taken out glass sample and is dried in vacuo.
Optionally, in step 1), the specific steps of grafted fluoropolymer surfactant are as follows: 1.3a) use fluorine-containing surfactants
Agent carries out immersion treatment to glass sample, takes out after reacting 72~168 hours under vacuum conditions, and it is dry to carry out vacuum after cleaning
It is dry.
Optionally, in step 1), the specific steps of grafted fluoropolymer surfactant are as follows: 1.3b) using dry toluene as solvent
3- isocyanide acyl propyl-dimethyl chlorosilane (ICPDMS) solution that compound concentration is 33% soaks the glass sample after activation processing
Bubble is in ICPDMS solution, under room temperature, vacuum anhydrous and oxygen-free environment, reacts 24 hours；Fluorine-containing surfactant is dissolved in again
In dry toluene, and MgSO is added4Water removal, then by glass sample be soaked in wherein, continue under vacuum conditions reaction 72~
It takes out after 168 hours, is dried in vacuo after cleaning.It is to utilize to contain isocyanic acid using the main purpose that ICPDMS solution is handled
Si-Cl on the chlorosilane of ester is easy to react with the O-H of glass surface, can be grafted upper isocyanates in glass surface
Group be conducive to further grafted fluoropolymer surface-active so that ICPDMS and glass surface react to form chemical bond company
Agent, since isocyanate groups are easy to hydrolyze, this experimentation must carry out in the environment of anhydrous and oxygen-free.
Preferably, in step 2), the effective power of sputtering plasma instrument is 500W~700W, is passed through the flow of discharge gas
For 0.5~0.8L/min, air pressure is 0.2~0.4 atmospheric pressure when electric discharge, and the processing time is 65~80min.
Preferably, in step 1), the fluorine-containing surfactant is that the water-soluble non-ionic fluorocarbon surface of ethoxy base class is living
Property agent, can be selected Du Pont FSN-100.
Preferably, in step 2), the discharge gas is non-polymerization gas, preferably non-reactive gas；Further
Preferably purity be 99.999% nitrogen and/or purity be 99.999% helium；When using 99.999% nitrogen and
When the mixed gas of 99.999% helium, it can be passed through simultaneously in 1:1 ratio.
Invention also provides a kind of hydrophobic antifog glass of oleophobic, surface is dredged for what is handled using the above method
Oily Hydrophobic glass coating.
Preferably, the surface microstructure of the oleophobic Hydrophobic glass coating is height fluctuating, the table with tapering protrusion
Face.
The beneficial effects of the present invention are: coating surface can be improved by the way that fluorine-containing coat is carried out plasma modification processing
Roughness, generate height rise and fall, the surface with tapering protrusion, and even particle distribution reaches nanoscale (5-10nm),
Modified coating surface increases the contact angle of water simultaneously, unobvious on the influence of the contact angle of oil, and drop has with film surface
Lesser contact area, surface energy is low, shows good hydrophobic oleophobic characteristic.Simple production process of the present invention, is processed into
This is low, and anti-fog performance is good, can be widely applied to the silicates glass such as glass for building purposes, windshield.
Detailed description of the invention
Fig. 1~2 are that the AFM that the carry out atomic force microscope of the hydrophobic antifog glass coating of oleophobic obtained is tested shines
Piece, wherein Fig. 1 is surface two-dimensional appearance phase, Fig. 2 is three-dimensional surface shape phase.
Fig. 3 is drop photo of the water on the hydrophobic antifog glass coating of oleophobic.
Fig. 4 is drop photograph of the hexadecane on the hydrophobic antifog glass coating of oleophobic.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below.
Embodiment 1:
Glass substrate is put into beaker, hydrogen peroxide and the concentrated sulfuric acid mixing washing lotion heat treatment being added thereto, beaker
Stop heating when middle bubble-free generates.It takes out glass substrate to be cooled to room temperature, is put into supersound washing in deionized water, be dried in vacuo
Processing meron, then fluorine-containing surfactant (FSN-100) immersion treatment for being 10% with weight ratio are obtained, under vacuum conditions
Reaction is taken out after 168 hours, is cleaned with ethyl alcohol and deionized water, is then dried in vacuo, obtains first step sample.
The glass sample with fluorine-containing coat surface of preparation is placed in again in the sample column of sputtering plasma instrument, is first taken out
Vacuum and with being passed through discharge gas, after air replace completely it is clean after start to discharge.Test use N:(purity 99.999%), He
(purity 99.999%) is tested (two kinds of gases are by 1:1 while being passed through) as discharge gas, and control discharge frequency exists
13.56MHz frequency band.Radio frequency plasma effective power is 400W in test, is passed through gas flow 0.4L/min, gas when electric discharge
Pressure is 0.1 atmospheric pressure, and the processing time is 40min, finally takes out and obtains required sample.
Embodiment 2:
Glass substrate is put into beaker, hydrogen peroxide and the concentrated sulfuric acid mixing washing lotion heat treatment being added thereto, beaker
Stop heating when middle bubble-free generates.It takes out glass substrate to be cooled to room temperature, is put into supersound washing in deionized water, be dried in vacuo
Processing meron, then fluorine-containing surfactant (FSN-100) immersion treatment for being 20% with weight ratio are obtained, under vacuum conditions
Reaction is taken out after 72 hours, is cleaned with ethyl alcohol and deionized water, is then dried in vacuo, obtains first step sample.
The glass sample with fluorine-containing coat surface of preparation is placed in sample column again, first vacuumizes and is put with being passed through
Electrical body starts to discharge after air is replaced completely completely.Test respectively select N:(purity 99.999%), He (purity
99.999%) it is tested (two kinds of gases are by 1:1 while being passed through) as discharge gas, control discharge frequency is in 13.56MHz frequency
Rate band.Radio frequency plasma effective power is 700W in test, is passed through gas flow 0.8L/min, and air pressure is 0.4 when electric discharge
Atmospheric pressure, processing time are 80min, finally take out and obtain required sample.
Embodiment 3:
Glass substrate is put into beaker, hydrogen peroxide and the concentrated sulfuric acid mixing washing lotion heat treatment being added thereto, beaker
Stop heating when middle bubble-free generates.It takes out glass substrate to be cooled to room temperature, is put into supersound washing in deionized water, be dried in vacuo
Processing meron, then fluorine-containing surfactant (FSN-100) immersion treatment for being 15% with weight ratio are obtained, under vacuum conditions
Reaction is taken out after 96 hours, is cleaned with ethyl alcohol and deionized water, is then dried in vacuo, obtains first step sample.
The glass sample with fluorine-containing coat surface of preparation is placed in sample column again, first vacuumizes and is put with being passed through
Electrical body starts to discharge after air is replaced completely completely.Test respectively select N:(purity 99.999%), He (purity
99.999%) it is tested (two kinds of gases are by 1:1 while being passed through) as discharge gas, control discharge frequency is in 13.56MHz frequency
Rate band.Radio frequency plasma effective power is 500W in test, is passed through gas flow 0.6L/min, and air pressure is 0.2 when electric discharge
Atmospheric pressure, processing time are 55min, finally take out and obtain required sample.
Embodiment 4:
Glass substrate is put into beaker, hydrogen peroxide and the concentrated sulfuric acid mixing washing lotion heat treatment being added thereto, beaker
Stop heating when middle bubble-free generates.It takes out glass substrate to be cooled to room temperature, is put into supersound washing in deionized water, be dried in vacuo
Processing meron, then fluorine-containing surfactant (FSN-100) immersion treatment for being 15% with weight ratio are obtained, under vacuum conditions
Reaction is taken out after 120 hours, is cleaned with ethyl alcohol and deionized water, is then dried in vacuo, obtains first step sample.
The glass sample with fluorine-containing coat surface of preparation is placed in sample column again, first vacuumizes and is put with being passed through
Electrical body starts to discharge after air is replaced completely completely.Test respectively select N:(purity 99.999%), He (purity
99.999%) it is tested (two kinds of gases are by 1:1 while being passed through) as discharge gas, control discharge frequency is in 13.56MHz frequency
Rate band.Radio frequency plasma effective power is 600W in test, is passed through gas flow 0.5L/min, and air pressure is 0.3 when electric discharge
Atmospheric pressure, processing time are 65min, finally take out and obtain required sample.
Embodiment 5:
Glass substrate is put into beaker, hydrogen peroxide and the concentrated sulfuric acid mixing washing lotion heat treatment being added thereto, beaker
Stop heating when middle bubble-free generates.It takes out glass substrate to be cooled to room temperature, is put into supersound washing in deionized water, be dried in vacuo
Processing meron, then fluorine-containing surfactant (FSN-100) immersion treatment for being 10% with weight ratio are obtained, under vacuum conditions
Reaction is taken out after 144 hours, is cleaned with ethyl alcohol and deionized water, is then dried in vacuo, obtains first step sample.
The glass sample with fluorine-containing coat surface of preparation is placed in sample column again, first vacuumizes and is put with being passed through
Electrical body starts to discharge after air is replaced completely completely.Test respectively select N:(purity 99.999%), He (purity
99.999%) it is tested (two kinds of gases are by 1:1 while being passed through) as discharge gas, control discharge frequency is in 13.56MHz frequency
Rate band.Radio frequency plasma effective power is 650W in test, is passed through gas flow 0.7L/min, and air pressure is 0.1 when electric discharge
Atmospheric pressure, processing time are 70min, finally take out and obtain required sample.
Embodiment 6:
Glass substrate is put into beaker, hydrogen peroxide and the concentrated sulfuric acid mixing washing lotion heat treatment being added thereto, beaker
Stop heating when middle bubble-free generates.It takes out glass substrate to be cooled to room temperature, is put into supersound washing in deionized water, be dried in vacuo
Processing meron is obtained, 3- isocyanide acyl propyl-dimethyl chlorosilane is reacted with the glass surface being activated, then with again
Amount is taken out after reacting 72 hours under vacuum conditions than fluorine-containing surfactant (FSN-100) immersion treatment for being 10%, uses second
Pure and mild deionized water is cleaned, and is then dried in vacuo, is obtained first step sample.
The glass sample with fluorine-containing coat surface of preparation is placed in sample column again, first vacuumizes and is put with being passed through
Electrical body starts to discharge after air is replaced completely completely.Test respectively select N:(purity 99.999%), He (purity
99.999%) it is tested (two kinds of gases are by 1:1 while being passed through) as discharge gas, control discharge frequency is in 13.56MHz frequency
Rate band.Radio frequency plasma effective power is 650W in test, is passed through gas flow 0.7L/min, and air pressure is 0.1 when electric discharge
Atmospheric pressure, processing time are 70min, finally take out and obtain required sample.
Validity check
Atomic force microscope test is carried out to the coating surface for the hydrophobic antifog glass of oleophobic that Examples 1 to 6 is handled,
Surface topography is as shown in Figure 1 and Figure 2.It can be seen from the figure that under relatively high amplification factor, by corona treatment
Fluorine-containing coat observes the microstructure of its coating, has more tapering convex meeting surface, more than simple fluorine-containing coat protrusion
To be sharp, and distribution density is thinner, and roughness increases, this makes water droplet and film surface have lesser contact area, surface
Energy is low, so showing hydrophobic property.And the particle composition of treated surface is nanometer scale, and distribution of particles
More uniformly, roughness is nanometer scale, can further decrease coating surface energy.In Fig. 1, color is indicated from dark color to light color
Height is from 0nm to 10nm, it can be seen that the height of most of protrusion particle is 5nm, and highest point is up to 10nm.
Hexadecane and water are dripped respectively on the hydrophobic antifog glass surface of oleophobic that embodiment is handled, directly observed
Drop its surface wet face state, as shown in Figure 3, Figure 4.Glass coating wettability after plasma modification is changed
Become, it can be clearly seen that, the wettability of water becomes hydrophobic state from hydrophily, and contact angle is increased to 92 ° from 30 °, hexadecane
Drop can achieve 70 ° in contact angle on surface of coating, which is rendered obvious by hydrophobic oil transportation characteristic.
Claims (6)
1. a kind of preparation method of the hydrophobic antifog glass coating of oleophobic, characterized by the following steps:
1) glass sample is activated, then grafted fluoropolymer surfactant on the glass surface, forms fluorine-containing coat, makes
Hydrophilic and oleophobic state is presented in glass surface；
Wherein, the specific steps of activation processing are as follows:
1.1) glass sample is immersed in the mixing washing lotion of hydrogen peroxide and the concentrated sulfuric acid and is heated, until bubble-free stops when generating
Heating；
1.2) it takes out glass sample to be cooled to room temperature, is put into supersound washing in deionized water, take out glass sample and carry out vacuum
It is dry；
The specific steps of grafted fluoropolymer surfactant are as follows:
1.3) the 3- isocyanide acyl propyl-dimethyl chlorosilane solution for being 33% as solvent compound concentration using dry toluene, at activation
Glass sample after reason is immersed in 3- isocyanide acyl propyl-dimethyl chlorosilane solution, under room temperature, vacuum anhydrous and oxygen-free environment,
Reaction 24 hours；Fluorine-containing surfactant is dissolved in dry toluene again, and MgSO is added4Water removal, then soaks glass sample
It steeps in wherein, continuing to take out after reacting 72~168 hours under vacuum conditions, is dried in vacuo after cleaning；
2) plasma etching treatment is carried out to the glass sample surface by step 1) processing using sputtering plasma instrument to obtain
The hydrophobic antifog glass coating of oleophobic, the effective power of sputtering plasma instrument are 400W~700W, and discharge frequency control exists
13.56MHz frequency band, the flow for being passed through discharge gas is 0.4~0.8L/min, and air pressure is absolute pressure 0.1~0.4 big when electric discharge
Air pressure, processing time are 40~80min；
After handling above, glass surface forms the tapering protrusion that height rises and falls, grain diameter is 5~10nm, makes glass table
Hydrophobic oleophobic state is presented in face.
2. the preparation method of the hydrophobic antifog glass coating of oleophobic according to claim 1, it is characterised in that: the step 2)
In, the effective power of sputtering plasma instrument is 500W~700W, and the flow for being passed through discharge gas is 0.5~0.8L/min, electric discharge
When air pressure be 0.2~0.4 atmospheric pressure, the processing time be 65~80min.
3. the preparation method of the hydrophobic antifog glass coating of oleophobic according to claim 1, it is characterised in that: the step 1)
In, fluorine-containing surfactant is the non-ionic fluorocarbon surfactant of water-soluble ethoxy base class.
4. the preparation method of the hydrophobic antifog glass coating of oleophobic according to claim 1, it is characterised in that: the step 2)
In, discharge gas is non-polymerization gas.
5. the preparation method of the hydrophobic antifog glass coating of oleophobic according to claim 4, it is characterised in that: the step 2)
In, the mixture of discharge gas is the nitrogen that purity is 99.999% or purity is 99.999% helium or both.
6. a kind of hydrophobic antifog glass of oleophobic, it is characterised in that: the surface of the hydrophobic antifog glass of the oleophobic is using claim 1
The oleophobic Hydrophobic glass coating that the preparation method of the hydrophobic antifog glass coating of oleophobic described in any one of~5 is handled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610850662.7A CN106517813B (en) | 2016-09-26 | 2016-09-26 | The preparation method of the hydrophobic antifog glass of oleophobic and its coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610850662.7A CN106517813B (en) | 2016-09-26 | 2016-09-26 | The preparation method of the hydrophobic antifog glass of oleophobic and its coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106517813A CN106517813A (en) | 2017-03-22 |
| CN106517813B true CN106517813B (en) | 2019-09-24 |
Family
ID=58344282
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610850662.7A Active CN106517813B (en) | 2016-09-26 | 2016-09-26 | The preparation method of the hydrophobic antifog glass of oleophobic and its coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106517813B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109160739B (en) * | 2018-09-19 | 2021-09-03 | 河北新瑞能玻璃科技有限公司 | Method for preparing hydrophobic glass layer for building |
| CN109664493B (en) * | 2018-12-13 | 2020-07-10 | 华中科技大学 | An Efficient Plasma Method for Graphically Controlling Wettability of Functional Thin Films |
| DE102021107593A1 (en) | 2020-03-30 | 2021-09-30 | Schott Ag | Anti-glare glass articles and methods of making anti-glare glass articles |
| CN114121598A (en) * | 2020-09-01 | 2022-03-01 | 中国科学院大连化学物理研究所 | A Plasma-Assisted Surface Hydrophilic or Hydrophobic Modification Method |
| CN113716882B (en) * | 2021-09-06 | 2023-09-01 | 广东中融玻璃科技有限公司 | Processing Technology of Low-e Laminated Glass |
| CN113603371A (en) * | 2021-09-06 | 2021-11-05 | 广东中融玻璃科技有限公司 | Preparation method of colored glaze coated glass |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105217967A (en) * | 2015-09-28 | 2016-01-06 | 武汉钢铁(集团)公司 | A kind of formation method of glass antifogging anti coating |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1555249A1 (en) * | 2004-01-15 | 2005-07-20 | Nanogate Coating Systems GmbH | Hydrophobic and/or oleophobic coating on microstructured glass surfaces providing an anti-fingerprint effect |
| FR2982609B1 (en) * | 2011-11-16 | 2014-06-20 | Saint Gobain | HYDROPHOBIC GLAZING |
| CN103951278B (en) * | 2014-05-04 | 2015-12-09 | 江南大学 | A kind of superhydrophobic superoleophobic anti-reflection glass surface layer and preparation method thereof |
-
2016
- 2016-09-26 CN CN201610850662.7A patent/CN106517813B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105217967A (en) * | 2015-09-28 | 2016-01-06 | 武汉钢铁(集团)公司 | A kind of formation method of glass antifogging anti coating |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106517813A (en) | 2017-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106517813B (en) | The preparation method of the hydrophobic antifog glass of oleophobic and its coating | |
| Li et al. | Nonfluorinated, transparent, and spontaneous self-healing superhydrophobic coatings enabled by supramolecular polymers | |
| Shirgholami et al. | Fabrication of superhydrophobic polymethylsilsesquioxane nanostructures on cotton textiles by a solution–immersion process | |
| JP5962652B2 (en) | Antireflection glass substrate and method for producing antireflection glass substrate | |
| KR101100380B1 (en) | Surface treatment method for treating the surface of the substrate with high hydrophobicity | |
| Parale et al. | OTES modified transparent dip coated silica coatings | |
| TW201906800A (en) | Item with water dialing oil layer and manufacturing method thereof | |
| Cai et al. | Transparent superhydrophobic hollow films (TSHFs) with superior thermal stability and moisture resistance | |
| Nomeir et al. | Recent progress on transparent and self-cleaning surfaces by superhydrophobic coatings deposition to optimize the cleaning process of solar panels | |
| CN105855151A (en) | Long-acting hydrophobic-oleophobic surface treatment process | |
| JP2009515728A (en) | Super-hydrophilic or super-hydrophobic product, its production method and use of the product | |
| CN101270260A (en) | A kind of superhydrophobic surface coating material and preparation method thereof | |
| CN108752988A (en) | A kind of preparation method of super-hydrophobic silicon colloidal sol and super-hydrophobic coat | |
| CN111962049A (en) | Plasma chemical vapor deposition nano super-hydrophobic coating and preparation method thereof | |
| Salehi et al. | Antireflective and anti-dust modified silica based thin film on solar cell cover glass | |
| Wang et al. | Durable superhydrophobic coating based on inorganic/organic double-network polysiloxane and functionalized nanoparticles | |
| Liu et al. | Integrated super-hydrophobic and antireflective PDMS bio-templated from nano-conical structures of cicada wings | |
| KR101401754B1 (en) | Superhydrophobic coating solution composition and method for producing the coating composition | |
| Wang et al. | UV/ozone-assisted tribochemistry-induced nanofabrication on Si (100) surfaces | |
| WO2014061615A1 (en) | Production method for glass having anti-reflective properties, and glass having anti-reflective properties | |
| Topcu et al. | Preparation of stable, transparent superhydrophobic film via one step one pot sol-gel method | |
| JP7317203B2 (en) | SELF-HEALING OR REPEATABLE PRODUCTS, PRODUCTION METHOD AND APPLICATION THEREOF | |
| Wankhede et al. | Development of hydrophobic non-fluorine sol-gel coatings on aluminium using long chain alkyl silane precursor | |
| CN106833043A (en) | A kind of transparent durable super-hydrophobic new material coating and preparation method thereof | |
| Abu-Dheir et al. | Sol-gel coating of colloidal particles deposited glass surface pertinent to self-cleaning applications |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20170703 Address after: 430083, Hubei Wuhan Qingshan District Factory No. 2 Gate joint stock company organs Applicant after: Wuhan iron and Steel Company Limited Address before: 430083 Qingshan District, Hubei, Wuhan Applicant before: WUHAN IRON AND STEEL CORPORATION |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |