CN108384302A - A kind of compound anti-soil film and its prepare application method - Google Patents
A kind of compound anti-soil film and its prepare application method Download PDFInfo
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- CN108384302A CN108384302A CN201810175143.4A CN201810175143A CN108384302A CN 108384302 A CN108384302 A CN 108384302A CN 201810175143 A CN201810175143 A CN 201810175143A CN 108384302 A CN108384302 A CN 108384302A
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1693—Antifouling paints; Underwater paints as part of a multilayer system
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/24—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen halogen-containing groups
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Abstract
The present invention relates to a kind of compound anti-soil films, compound anti-soil film is coated on the surface of substrate material, including inorganic oxide film and fluorine silicon organic thin film, inorganic oxide film is coated on the surface of substrate material, fluorine silicon organic thin film is coated on inorganic oxide film, inorganic oxide film includes the aqueous solution and ethyl alcohol of nano silicon oxide and nano-titanium oxide, and the volume ratio of the aqueous solution and ethyl alcohol of nano silicon oxide and nano-titanium oxide is 1:4~1:9, fluorine silicon organic thin film includes fluorine silicon organic matter and hydrofluoroether, fluorine silicon organic matter is the solution for including fluoroalkyl ether and active silyl mixture, wherein fluoroalkyl ether includes nine fluoro butyl ether of ethyl perfluorobutyl ether and ethyl, the content of ethyl perfluorobutyl ether is 40 ~ 50%, the content of nine fluoro butyl ether of ethyl is 30 ~ 40%, and remaining content is silicyl organic matter, and the volume ratio of fluorine silicon organic matter and hydrofluoroether is 1:500~1:1000.
Description
Technical field
The present invention relates to antifouling thin film technique field more particularly to a kind of compound anti-soil film and its prepare application method.
Background technology
Hydrophobic, oleophobic material can form thin film in the outer surface of substrate material, its surface is made to can significantly reduce, from
And show pollution-free, low frictional properties, hydrophobic and oleophobic characteristic.Hydrophobic oleophobic film has important work in daily life
With, including printing and dyeing, food packaging, construction material and antifouling preservation antioxidation etc..
The wetability of the surface of solids is codetermined by its chemical composition and microstructure.In general, the change on its surface
The wettability of the surface of the pairs of solid of group plays decisive role.Therefore the low surface energy film of hydrophobic oleophobic is prepared, it is first
First to select low-surface-energy material.Wherein, fluorine silicon organic material is most common hydrophobic oleophobic film preparation material.Organic fluorinated silicone
Material intersects material as organosilicon and Organic fluoride, and properties of product have taken into account the characteristic of organosilicon product and Organic fluoride product, tool
There is the features such as low surface tension, solvent resistant and chemical-resistance.But organic fluorinated silicone material preparation is used alone in substrate surface
Film, water contact angle degree can only achieve 110 °, and use, when RF magnetron sputtering material surface, water contact angle then can only
Reach 100 ° or so.Therefore surface free energy is adjusted only with the method for changing chemical composition on smooth surface, it is difficult to obtain
Obtain higher water contact angle.Reach higher contact angle, just must both consider the chemical composition of the surface of solids, also to consider
The microstructure on surface.
The preparation application method of anti-soil film includes mainly chemical vapour deposition technique, electrochemical deposition method, sol-gel
Method, magnetron sputtering method and plasma spraying method etc..Or but these methods using expensive material or need to use
Special process equipment such as magnetron sputtering process equipment or plasma processing equipment, thus cost is higher.Because of the invention one kind
Simple and low manufacturing cost hydrophobic oleophobic film is necessary.
Invention content
In view of this, it is necessary to provide a kind of compound anti-soil film that can be solved the above problems and its preparing application method.
The invention is realized in this way the present invention provides a kind of compound anti-soil film, the compound anti-soil film is coated in lining
On the surface of bottom material, it is characterised in that：Including inorganic oxide film and fluorine silicon organic thin film, the inorganic oxide film applies
It overlays on the surface of substrate material, the fluorine silicon organic thin film is coated on inorganic oxide film.
The inorganic oxide film includes：
Reagent：The aqueous solution of nano silicon oxide and nano-titanium oxide.
Dispensing reagents agent：Ethyl alcohol.
The mass fraction of titanium oxide in the aqueous solution of the nano silicon oxide and nano-titanium oxide is 0.3 ~ 0.6%, oxidation
The content of silicon is 0.05 ~ 0.1%, and the grain size of nano silicon oxide and nano-titanium oxide is 10 ~ 50nm, the nano silicon oxide and is received
The aqueous solution of rice titanium oxide and the volume ratio of ethyl alcohol are 1:4~1:9.
The fluorine silicon organic thin film includes：
Reagent：Fluorine silicon organic matter.
Dispensing reagents agent：Hydrofluoroether.
The fluorine silicon organic matter is the solution for including fluoroalkyl ether and active silyl mixture, wherein fluoroalkyl ether packet
Nine fluoro butyl ether of ethyl perfluorobutyl ether and ethyl is included, the content of the ethyl perfluorobutyl ether is 40 ~ 50%, nine fluorine of ethyl
Content for butyl ether is 30 ~ 40%, and remaining content is silicyl organic matter, the fluorine silicon organic matter and the hydrofluoroether
Volume ratio is 1:500~1:1000.
Further, the grain size of the nano silicon oxide and nano-titanium oxide is 30nm.
Further, the volume ratio of the aqueous solution and ethyl alcohol of the nano silicon oxide and nano-titanium oxide is 1:6.
Further, the content of the ethyl perfluorobutyl ether is 45%, and the content of nine fluoro butyl ether of ethyl is 35%, first
The content of silylation organic matter is 20%.
The present invention also provides the preparation application methods of above-mentioned compound anti-soil film, are as follows：
Step 1：The cleaning of substrate material.
The substrate material for coating the compound anti-soil film will be needed to be placed in neutral cleaning solution first, is cleaned by ultrasonic 30 points
Clock, the sample after ultrasonic cleaning are rinsed using clear water first, are then positioned over again in distilled water and are continued to be cleaned by ultrasonic 15 minutes, surpass
Substrate material is taken out after sound, is placed in baking oven and is dried using isopropanol flushing substrate material surface.
Step 2：Prepare simultaneously coating inorganic oxidation film.
The aqueous solution of nano silicon oxide and nano-titanium oxide is uniformly mixed with ethyl alcohol according to volume ratio, will be mixed molten
Liquid injects in spray gun, and uniform spraying plating is on the surface of substrate material under the drive of carrier gas.
Step 3：It is oxide curing.
Substrate material after spraying plating irradiates 15-25min in the UV lamp, by oxide curing on the surface of substrate.
Step 4：It prepares and coats fluorine silicon organic thin film.
Fluorine silicon organic matter is uniformly mixed with hydrofluoroether according to volume ratio, in mixed agent transfer to spray gun, normal
Mix reagent is continued under temperature on the solidification oxide on the surface of substrate of the spraying plating in step 3.
Step 5：High temperature is dried.
The substrate material of the reagent of spraying plating of step 4 kind is placed in baking oven, and is warming up to 90 ~ 120 DEG C, constant temperature baking
30min, the coating layer thickness after baking are 100 ~ 200nm.
Step 6：Plasma treatment.
By in step 5, the substrate material after toasting is placed in Surface Treatment with Plasma instrument, the fluorinated organic compound on surface
It will continue to be crosslinked.
The advantages of a kind of compound anti-soil film provided by the invention and its preparation application method, is：Including inorganic oxide film
With fluorine silicon organic thin film, which is the combination of inorganic oxide and fluorine silicon organic matter, first in substrate
Surface introduces inorganic oxide nano particle, which is solidificated in the surface of substrate material under the action of ultraviolet light, changes
The architectural characteristic of substrate surface, that is, the aqueous solution for disperseing Nano particles of silicon dioxide and titanium dioxide nano-particle, to lining
Bottom be tentatively modified, and the nanometer oxide particle has large specific surface area, and adsorption capacity is strong, is easily dispersed, and has
Excellent chemical stability, while the silicon dioxide plasma of Surface Creation absorb air in silicon fluoride of the spraying plating on surface
In water hydrolyze, and again the fluorine silicon organic matter of spraying plating by hydrolysis be grafted on the surface of nano-particle, utilize simultaneously
The self-assembling function of fluorine silicon organic matter, spontaneously forms orderly monolayer on interface, to obtain the antifouling of low-surface-energy
Film.
The hydrophobic and oleophobic performance of the laminated film is significantly improved, and preparation method is simple.In substrate
Surface spraying plating first prepares inorganic oxide film, can effectively improve the architectural characteristic of substrate surface, changes the coarse journey on surface
Degree；The laminated film is prepared using the method for spraying plating simultaneously, technological process process is simple, and the requirement to equipment is relatively low, reduces
Production cost is suitble to large-scale production to prepare.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
A kind of compound anti-soil film, the compound anti-soil film is coated on the surface of substrate material, including inorganic oxide film
With fluorine silicon organic thin film, the inorganic oxide film is coated on the surface of substrate material, and the fluorine silicon organic thin film applies
It overlays on inorganic oxide film.
The inorganic oxide film includes：
Reagent：The aqueous solution of nano silicon oxide and nano-titanium oxide.
Dispensing reagents agent：Ethyl alcohol.
The mass fraction of titanium oxide in the aqueous solution of the nano silicon oxide and nano-titanium oxide is 0.3 ~ 0.6%, oxidation
The content of silicon is 0.05 ~ 0.1%, and the grain size of nano silicon oxide and nano-titanium oxide is 30nm, the nano silicon oxide and nano oxygen
The volume ratio of the aqueous solution and ethyl alcohol of changing titanium is 1:6.
The fluorine silicon organic thin film includes：
Reagent：Fluorine silicon organic matter.
Dispensing reagents agent：Hydrofluoroether.
The fluorine silicon organic matter is the solution for including fluoroalkyl ether and active silyl mixture, wherein fluoroalkyl ether packet
Nine fluoro butyl ether of ethyl perfluorobutyl ether and ethyl is included, the content of the ethyl perfluorobutyl ether is 45%, nine fluoro fourth of ethyl
The content of base ether is 35%, and the content of silicyl organic matter is 20%, the volume ratio of the fluorine silicon organic matter and the hydrofluoroether
It is 1:500.
The present invention also provides the preparation application methods of above-mentioned compound anti-soil film, are as follows：
Step 1：The cleaning of substrate material.
The substrate material for coating the compound anti-soil film will be needed to be placed in neutral cleaning solution first, is cleaned by ultrasonic 30 points
Clock, the sample after ultrasonic cleaning are rinsed using clear water first, are then positioned over again in distilled water and are continued to be cleaned by ultrasonic 15 minutes, surpass
Substrate material is taken out after sound, is placed in baking oven and is dried using isopropanol flushing substrate material surface.
Step 2：Prepare simultaneously coating inorganic oxidation film.
The aqueous solution of nano silicon oxide and nano-titanium oxide is uniformly mixed with ethyl alcohol according to volume ratio, will be mixed molten
Liquid injects in spray gun, and uniform spraying plating is on the surface of substrate material under the drive of carrier gas.
Step 3：It is oxide curing.
Substrate material after spraying plating irradiates 15-25min in the UV lamp, by oxide curing on the surface of substrate.
Step 4：It prepares and coats fluorine silicon organic thin film.
Fluorine silicon organic matter is uniformly mixed with hydrofluoroether according to volume ratio, in mixed agent transfer to spray gun, normal
Mix reagent is continued under temperature on the solidification oxide on the surface of substrate of the spraying plating in step 3.
Step 5：High temperature is dried.
The substrate material of the reagent of spraying plating of step 4 kind is placed in baking oven, and is warming up to 90 ~ 120 DEG C, constant temperature baking
30min, the coating layer thickness after baking are 100 ~ 200nm.
Step 6：Plasma treatment.
By in step 5, the substrate material after toasting is placed in Surface Treatment with Plasma instrument, the fluorinated organic compound on surface
It will continue to be crosslinked.
After step 5 processing, 115 ° of the water contact angle average out to of substrate surface, slide angle is 40 ° or so, passes through step
After six processing, the water contact angle on the surface of substrate material can reach 123 °, and the contact angle of oleic acid can also reach 70 °.
The advantages of a kind of compound anti-soil film provided by the invention and its preparation application method, is：Including inorganic oxide film
With fluorine silicon organic thin film, which is the combination of inorganic oxide and fluorine silicon organic matter, first in substrate
Surface introduces inorganic oxide nano particle, which is solidificated in the surface of substrate material under the action of ultraviolet light, changes
The architectural characteristic of substrate surface, that is, the aqueous solution for disperseing Nano particles of silicon dioxide and titanium dioxide nano-particle, to lining
Bottom be tentatively modified, and the nanometer oxide particle has large specific surface area, and adsorption capacity is strong, is easily dispersed, and has
Excellent chemical stability, while the silicon dioxide plasma of Surface Creation absorb air in silicon fluoride of the spraying plating on surface
In water hydrolyze, and again the fluorine silicon organic matter of spraying plating by hydrolysis be grafted on the surface of nano-particle, utilize simultaneously
The self-assembling function of fluorine silicon organic matter, spontaneously forms orderly monolayer on interface, to obtain the antifouling of low-surface-energy
Film.
The hydrophobic and oleophobic performance of the laminated film is significantly improved, and preparation method is simple.In substrate
Surface spraying plating first prepares inorganic oxide film, can effectively improve the architectural characteristic of substrate surface, changes the coarse journey on surface
Degree；The laminated film is prepared using the method for spraying plating simultaneously, technological process process is simple, and the requirement to equipment is relatively low, reduces
Production cost is suitble to large-scale production to prepare.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (5)
1. a kind of compound anti-soil film, the compound anti-soil film is coated on the surface of substrate material, it is characterised in that：Including inorganic
Oxidation film and fluorine silicon organic thin film, the inorganic oxide film are coated on the surface of substrate material, and the fluorine silicon is organic
Object thin film coated is on inorganic oxide film；
The inorganic oxide film includes：
Reagent：The aqueous solution of nano silicon oxide and nano-titanium oxide；
Dispensing reagents agent：Ethyl alcohol；
The mass fraction of titanium oxide in the aqueous solution of the nano silicon oxide and nano-titanium oxide is 0.3 ~ 0.6%, silica
Content is 0.05 ~ 0.1%, and the grain size of nano silicon oxide and nano-titanium oxide is 10 ~ 50nm, the nano silicon oxide and nano oxygen
The volume ratio of the aqueous solution and ethyl alcohol of changing titanium is 1:4~1:9；
The fluorine silicon organic thin film includes：
Reagent：Fluorine silicon organic matter；
Dispensing reagents agent：Hydrofluoroether；
The fluorine silicon organic matter is the solution for including fluoroalkyl ether and active silyl mixture, and wherein fluoroalkyl ether includes second
The content of nine fluoro butyl ether of base perfluorobutyl ether and ethyl, the ethyl perfluorobutyl ether is 40 ~ 50%, nine fluoro fourth of ethyl
The content of base ether is 30 ~ 40%, and remaining content is silicyl organic matter, the volume of the fluorine silicon organic matter and the hydrofluoroether
Than being 1:500~1:1000.
2. a kind of compound anti-soil film according to claim 1, which is characterized in that the nano silicon oxide and nano-titanium oxide
Grain size be 30nm.
3. a kind of compound anti-soil film according to claim 1, which is characterized in that the nano silicon oxide and nano-titanium oxide
Aqueous solution and ethyl alcohol volume ratio be 1:6.
4. a kind of compound anti-soil film according to claim 1, which is characterized in that the content of the ethyl perfluorobutyl ether is
45%, the content of nine fluoro butyl ether of ethyl is 35%, and the content of silicyl organic matter is 20%.
5. a kind of compound anti-soil film according to claim 1 ~ 4 any one, which is characterized in that it prepares application method
For：
Step 1：The cleaning of substrate material；
The substrate material for coating the compound anti-soil film will be needed to be placed in neutral cleaning solution first, be cleaned by ultrasonic 30 minutes, surpassed
Sample after sound cleaning is rinsed using clear water first, is then positioned over again in distilled water and is continued to be cleaned by ultrasonic 15 minutes, ultrasound knot
Substrate material is taken out after beam, is placed in baking oven and is dried using isopropanol flushing substrate material surface；
Step 2：Prepare simultaneously coating inorganic oxidation film；
The aqueous solution of nano silicon oxide and nano-titanium oxide is uniformly mixed with ethyl alcohol according to volume ratio, mixed solution is noted
Enter in spray gun, uniform spraying plating is on the surface of substrate material under the drive of carrier gas；
Step 3：It is oxide curing；
Substrate material after spraying plating irradiates 15-25min in the UV lamp, by oxide curing on the surface of substrate；
Step 4：It prepares and coats fluorine silicon organic thin film；
Fluorine silicon organic matter is uniformly mixed with hydrofluoroether according to volume ratio, in mixed agent transfer to spray gun, at normal temperatures
Mix reagent is continued on the solidification oxide on the surface of substrate of the spraying plating in step 3；
Step 5：High temperature is dried；
The substrate material of the reagent of spraying plating of step 4 kind is placed in baking oven, and is warming up to 90 ~ 120 DEG C, constant temperature baking
30min, the coating layer thickness after baking are 100 ~ 200nm；
Step 6：Plasma treatment；
By in step 5, the substrate material after toasting is placed in Surface Treatment with Plasma instrument, and the fluorinated organic compound on surface will be after
Continuous crosslinking.
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| CN201810175143.4A CN108384302A (en) | 2018-03-02 | 2018-03-02 | A kind of compound anti-soil film and its prepare application method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040221A (en) * | 2019-02-20 | 2020-04-21 | 中国科学院宁波材料技术与工程研究所 | Antibacterial self-cleaning film and preparation method and application thereof |
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| CN102702553A (en) * | 2012-06-29 | 2012-10-03 | 山东轻工业学院 | Method for preparing inorganic particle/epoxy resin super hydrophobic film |
| CN103909699A (en) * | 2013-01-08 | 2014-07-09 | 鸿富锦精密工业（深圳）有限公司 | Coated member and making method thereof |
| CN105176342A (en) * | 2015-10-08 | 2015-12-23 | 厦门博恩思应用材料科技有限公司 | Nano antibacterial and anti-fingerprint solution material as well as preparation method and application thereof |
| KR20170050320A (en) * | 2015-10-30 | 2017-05-11 | 주식회사 소프스톤 | hydrophobic and superhydrophobic coating layer and method of the same |
-
2018
- 2018-03-02 CN CN201810175143.4A patent/CN108384302A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702553A (en) * | 2012-06-29 | 2012-10-03 | 山东轻工业学院 | Method for preparing inorganic particle/epoxy resin super hydrophobic film |
| CN103909699A (en) * | 2013-01-08 | 2014-07-09 | 鸿富锦精密工业（深圳）有限公司 | Coated member and making method thereof |
| CN105176342A (en) * | 2015-10-08 | 2015-12-23 | 厦门博恩思应用材料科技有限公司 | Nano antibacterial and anti-fingerprint solution material as well as preparation method and application thereof |
| KR20170050320A (en) * | 2015-10-30 | 2017-05-11 | 주식회사 소프스톤 | hydrophobic and superhydrophobic coating layer and method of the same |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040221A (en) * | 2019-02-20 | 2020-04-21 | 中国科学院宁波材料技术与工程研究所 | Antibacterial self-cleaning film and preparation method and application thereof |
| CN111040221B (en) * | 2019-02-20 | 2022-06-03 | 中国科学院宁波材料技术与工程研究所 | Antibacterial self-cleaning film and preparation method and application thereof |
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Application publication date: 20180810 |