CN111925131A - Coated glass with surface self-cleaning function - Google Patents
Coated glass with surface self-cleaning function Download PDFInfo
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- CN111925131A CN111925131A CN202010632669.8A CN202010632669A CN111925131A CN 111925131 A CN111925131 A CN 111925131A CN 202010632669 A CN202010632669 A CN 202010632669A CN 111925131 A CN111925131 A CN 111925131A
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- glass substrate
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- 239000011521 glass Substances 0.000 title claims abstract description 163
- 238000004140 cleaning Methods 0.000 title claims abstract description 66
- 238000000576 coating method Methods 0.000 claims abstract description 111
- 239000011248 coating agent Substances 0.000 claims abstract description 104
- 239000000758 substrate Substances 0.000 claims abstract description 101
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 77
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 10
- 239000010410 layer Substances 0.000 claims description 88
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 84
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 51
- 238000003756 stirring Methods 0.000 claims description 48
- 239000000499 gel Substances 0.000 claims description 34
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 29
- 230000000873 masking effect Effects 0.000 claims description 26
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 25
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 25
- 239000002994 raw material Substances 0.000 claims description 23
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 20
- 229920002472 Starch Polymers 0.000 claims description 19
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 19
- 239000002518 antifoaming agent Substances 0.000 claims description 19
- 239000003755 preservative agent Substances 0.000 claims description 19
- 230000002335 preservative effect Effects 0.000 claims description 19
- 239000008107 starch Substances 0.000 claims description 19
- 235000019698 starch Nutrition 0.000 claims description 19
- KKYDYRWEUFJLER-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,10,10,10-heptadecafluorodecyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F KKYDYRWEUFJLER-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- 229920001187 thermosetting polymer Polymers 0.000 claims description 16
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 14
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 14
- 239000003431 cross linking reagent Substances 0.000 claims description 12
- 238000001723 curing Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000012790 adhesive layer Substances 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229920002120 photoresistant polymer Polymers 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 238000013035 low temperature curing Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- -1 2, 3-epoxypropoxy Chemical group 0.000 claims 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims 1
- 230000003075 superhydrophobic effect Effects 0.000 abstract description 16
- 238000013461 design Methods 0.000 abstract description 2
- 238000002834 transmittance Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 94
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 238000006136 alcoholysis reaction Methods 0.000 description 4
- 239000005348 self-cleaning glass Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000005344 low-emissivity glass Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001200 Ferrotitanium Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- XPBBUZJBQWWFFJ-UHFFFAOYSA-N fluorosilane Chemical compound [SiH3]F XPBBUZJBQWWFFJ-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 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
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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
- C03C17/34—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
Abstract
The invention discloses coated glass with a self-cleaning surface, which comprises a glass substrate, wherein the glass substrate can be any conventional transparent glass substrate in the field of solar photovoltaic glass, and is preferably an ultrawhite rolled glass substrate; one side of the glass substrate is coated with a layer of antireflection film, and the antireflection film is a silicon dioxide film layer, so that the transmittance of the coated glass can be effectively improved; the self-cleaning coating is a super-hydrophobic coating, can effectively improve the self-cleaning performance of the coated glass, and has higher practicability. The technical scheme has the advantages of reasonable process design and simple operation, not only effectively improves the bonding performance between the self-cleaning coating and the antireflection film and prolongs the service life of the coated glass, but also effectively improves the super-hydrophobic performance and the self-cleaning performance of the coated glass by modifying the silicon dioxide gel to form a super-hydrophobic plane on the surface of the coated glass.
Description
Technical Field
The invention relates to the technical field of coated glass, in particular to coated glass with a self-cleaning surface.
Background
Coated glass, also known as reflective glass. The coated glass is prepared by coating one or more layers of metal, alloy or metal compound films on the surface of glass to change the optical performance of the glass and meet certain specific requirements. The coated glass can be divided into the following types according to different characteristics of products: heat reflective glass, Low emissivity glass (Low-E), conductive film glass, and the like.
The heat reflection glass is generally formed by plating one or more layers of thin films composed of metals such as chromium, titanium or stainless steel or compounds thereof on the surface of the glass, so that the product has rich colors, has proper transmissivity to visible light, higher reflectivity to infrared rays and higher absorptivity to ultraviolet rays, is also called as sunlight control glass and is mainly used for buildings and glass curtain walls; the low-radiation glass is a film system formed by plating a plurality of layers of metals such as silver, copper or tin or compounds thereof on the surface of the glass, has higher transmissivity to visible light and higher reflectivity to infrared rays, has good heat-insulating property, is mainly used for buildings, automobiles, ships and other vehicles, and is generally made into hollow glass for use due to the poor strength of the film layer; the conductive film glass is formed by coating a conductive film such as indium tin oxide on the surface of glass, and can be used for heating, defrosting and defogging of glass, and can be used for liquid crystal display screens and the like.
At present, there is also a glass with high concern as self-cleaning glass, that is, self-cleaning effect is realized by a super-hydrophobic surface or a super-hydrophilic surface, but at present, self-cleaning glass on the market has short service life, the self-cleaning coating on the surface of the glass is not in close contact with an anti-reflection film, and the adhesion is poor, which brings great inconvenience to people.
In view of the above situation, we have designed a coated glass with self-cleaning surface and its preparation method. This is one of the problems that we are demanding to solve.
Disclosure of Invention
The invention aims to provide coated glass with a self-cleaning surface and a preparation method thereof, which aim to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the coated glass with the self-cleaning surface comprises a glass substrate, an antireflection film and a self-cleaning coating, wherein the antireflection film is coated on the surface of one side of the glass substrate, and the self-cleaning coating is coated on the antireflection film; the thickness of the antireflection film is 50-100nm, and the thickness of the self-cleaning coating is 100-200 nm.
The invention discloses coated glass with a self-cleaning surface and a preparation method thereof, wherein the coated glass comprises a glass substrate, the glass substrate can be any conventional transparent glass substrate in the field of solar photovoltaic glass, and is preferably an ultra-white rolled glass substrate; one side of the glass substrate is coated with a layer of antireflection film, and the antireflection film is a silicon dioxide film layer, so that the transmittance of the coated glass can be effectively improved; the self-cleaning coating is a super-hydrophobic coating, can effectively improve the self-cleaning performance of the coated glass, and has higher practicability.
Preferably, the self-cleaning coating comprises an adhesive layer and a modified silica gel layer, wherein the adhesive layer is coated on the antireflection film, and the modified silica gel layer is coated on the adhesive layer; the thickness of the bonding layer is 50-100nm, and the thickness of the modified silica gel layer is 50-100 nm.
The self-cleaning coating comprises a bonding layer and a modified silicon dioxide gel layer, and as is well known, when the coated glass is prepared, the surface of the coated glass is generally coated with an antireflection film firstly, and then the self-cleaning coating on the surface is coated, however, the self-cleaning coating in the technical scheme is selected to be a super-hydrophobic coating, and the bonding force between the super-hydrophobic coating and the antireflection film is poor when the super-hydrophobic coating is coated; after the coated glass is used for a period of time, the super-hydrophobic coating is easy to fall off, so that the self-cleaning performance of the coated glass is reduced; to the problem, the self-cleaning coating is designed to be an adhesive layer and a modified silica gel layer which are combined with each other, the adhesive layer is coated on the surface of the glass substrate, the modified silica gel layer is coated above the adhesive layer, and the modified silica gel layer is used as a super-hydrophobic coating, so that the adhesive layer can become a connecting bridge between the modified silica gel layer and the glass substrate, and the self-cleaning coating is more closely connected with the glass substrate.
Preferably, the modified silica gel layer comprises the following raw material components: by weight, 15-25 parts of tetraethyl silicate, 10-20 parts of ethanol, 20-40 parts of ammonia water, 5-15 parts of heptadecafluorodecyltrimethoxysilane and 3-8 parts of a cross-linking agent.
The raw materials of the modified silica gel layer in the technical scheme comprise tetraethyl silicate, ethanol, ammonia water, heptadecafluorodecyltrimethoxysilane and a cross-linking agent, wherein the tetraethyl silicate, the ethanol and the ammonia water can be used for preparing silica gel by a sol-gel method to form a super-hydrophobic surface, and then fluorosilane and the cross-linking agent are added for modification, so that the silica gel is modified in a hydrophobic manner, a rough surface structure is constructed, the surface energy of a coating is reduced, and the super-hydrophobicity of the modified silica gel layer is further improved.
Preferably, each raw material component of the bonding layer comprises: 8-16 parts of methanol, 15-30 parts of vinyl acetate, 5-10 parts of sodium hydroxide, 5-12 parts of aluminum sulfate, 3-5 parts of defoaming agent, 3-6 parts of preservative and 2-6 parts of starch.
In the technical scheme, the raw materials of the bonding layer comprise methanol, vinyl acetate, sodium hydroxide, aluminum sulfate, a defoaming agent, a preservative and starch; the polyvinyl alcohol can be prepared by designing methanol, vinyl acetate and sodium hydroxide, and the polyvinyl alcohol is generated after the vinyl acetate is subjected to alcoholysis in an alkaline environment of sodium hydroxide; the reason why the existing polyvinyl alcohol is not adopted and the polyvinyl alcohol is prepared by vinyl acetate alcoholysis is that acetic acid can be produced in vinyl acetate alcohol, and the surface of the antireflection film can be corroded to form a rough surface in the environments of sodium hydroxide and acetic acid, so that the binding force between the bonding layer and the antireflection film can be further improved, and the stability of the self-cleaning coating is ensured; meanwhile, aluminum sulfate, the defoaming agent, the preservative, the starch and the generated polyvinyl alcohol can react with each other to form a sticky bonding layer, so that the modified silicon dioxide gel layer and the antireflection film are tightly combined.
Preferably, the cross-linking agent is gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane.
Preferably, the preparation method of the coated glass with the self-cleaning surface comprises the following steps:
1) preparing raw materials;
2) coating an antireflection film;
3) coating a mask film on the side not coated with the antireflection film;
4) coating a self-cleaning coating on the antireflection film;
a) coating a bonding layer;
b) coating a modified silica gel layer;
5) removing the masking film;
6) and finishing the operation.
Preferably, the method comprises the following steps:
1) preparing raw materials;
a) weighing tetraethyl silicate, ethanol, ammonia water, heptadecafluorodecyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane according to a proportion for later use;
b) weighing methanol, vinyl acetate, sodium hydroxide, aluminum sulfate, a defoaming agent, a preservative and starch according to a proportion for later use;
c) cleaning the glass substrate for later use;
2) coating of an antireflection film: taking the cleaned glass substrate in the step 1), coating an antireflection film liquid on the surface of one side of the glass substrate by using a roll coating method, and curing at a low temperature to form an antireflection film;
3) coating a layer of photoresist on one side of the glass substrate which is not coated with the antireflection film after the glass substrate is treated in the step 2), and baking to solidify the masking film to form a masking film;
4) coating of the self-cleaning coating:
a) preparation of polyvinyl alcohol:
A. taking the methanol prepared in the step 1), putting the methanol into a four-neck flask, adding a sodium hydroxide solution, and starting a stirrer to stir;
B. putting the vinyl acetate prepared in the step 1) into a dropping funnel, slowly dropping the vinyl acetate into a four-neck flask within 25-35min, and stirring for reaction to obtain a first material;
b) coating of the bonding layer:
A. pouring the first material after the reaction in the step a) into a beaker, putting the glass substrate treated in the step 3) into the beaker, heating to 40-50 ℃, and reacting;
B. heating the beaker treated in the step A to 80-90 ℃, stirring at a constant temperature, sequentially adding the aluminum sulfate, the starch, the defoaming agent and the preservative prepared in the step 1) into the beaker, stirring, cooling to room temperature, forming a bonding layer on the surface of the glass substrate, and taking out the glass substrate for later use;
c) coating of the modified silica gel layer:
A. putting tetraethyl silicate and ethanol prepared in the step 1) into a beaker, performing magnetic stirring at room temperature, slowly dropwise adding ammonia water prepared in the step 1) into the beaker in the stirring process, continuing stirring after dropwise adding the ammonia water, and standing and aging after stirring to obtain silicon dioxide gel;
B. diluting the heptadecafluorodecyltrimethoxysilane and the gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane prepared in the step 1) with ethanol, sequentially putting into the beaker in the step A, and ultrasonically stirring to obtain modified silica gel;
C. placing the glass substrate treated in the step a) on a whirl coating platform, enabling the side which is not coated with the masking film to face downwards, uniformly dropwise adding the modified silica gel prepared in the step B, whirl coating for 1-2min, and then placing the glass substrate on a hot plate to heat for 2-4 min; repeatedly throwing the gel for 3-5 times, and then putting the gel into an oven for thermosetting to form a modified silicon dioxide gel layer;
5) removing the masking film: taking the glass substrate treated in the step 4), removing the mask film on one side of the glass substrate, and then cleaning with deionized water;
6) and finishing the operation.
Preferably, the method comprises the following steps:
1) preparing raw materials;
a) weighing tetraethyl silicate, ethanol, ammonia water, heptadecafluorodecyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane according to a proportion for later use;
b) weighing methanol, vinyl acetate, sodium hydroxide, aluminum sulfate, a defoaming agent, a preservative and starch according to a proportion for later use;
c) cleaning the glass substrate for later use; preparing raw materials required in the subsequent operation in the step 1), cleaning the glass substrate, removing oil stains on the surface of the glass substrate, and keeping the surface of the glass substrate dry, so as to prepare for the subsequent operation;
2) coating of an antireflection film: taking the cleaned glass substrate in the step 1), coating an antireflection film liquid on the surface of one side of the glass substrate by using a roll coating method, and curing at a low temperature to form an antireflection film; coating an antireflection film on one side of the glass substrate in the step 2), and coating by using a roll coating method, or coating by using a spraying method in actual operation;
3) coating a layer of photoresist on one side of the glass substrate which is not coated with the antireflection film after the glass substrate is treated in the step 2), and baking to solidify the masking film to form a masking film; wherein the baking temperature is 95-100 ℃, and the baking time is 15-20 min; coating photoresist on one side of the glass substrate, which is not coated with the antireflection film, in the step 3), forming a masking film after curing, wherein the masking film can play a role in protection, so that the situation that when the self-cleaning coating is coated, the side, which is not required to be processed, of the glass substrate is also coated with the self-cleaning coating is avoided, and the smooth proceeding of subsequent operation is ensured;
4) coating of the self-cleaning coating:
a) preparation of polyvinyl alcohol:
A. taking the methanol prepared in the step 1), putting the methanol into a four-neck flask provided with a stirrer, a condenser pipe, a thermometer and a dropping funnel, adding a sodium hydroxide solution, starting the stirrer to stir for 2-5 min;
B. putting the vinyl acetate prepared in the step 1) into a dropping funnel, slowly dropping the vinyl acetate into a four-neck flask within 25-35min, and stirring for reacting for 1.5-2.5h to obtain a first material; coating the self-cleaning coating in the step 4), firstly, alcoholysis is carried out on vinyl acetate in an alkaline environment by using methanol as an alcoholysis agent and sodium hydroxide as a catalyst to generate polyvinyl alcohol;
b) coating of the bonding layer:
A. pouring the first material after the reaction in the step a) into a beaker, putting the glass substrate treated in the step 3) into the beaker, heating to 40-50 ℃, and reacting for 15-25 min; in the step A, after polyvinyl alcohol is produced, sodium hydroxide solution and generated acetic acid are remained in the four-mouth flask, and the glass substrate is placed in the residual liquid, so that a rough surface can be formed on the antireflection film of the glass substrate, and the bonding layer and the antireflection film are more tightly bonded when the bonding layer is coated subsequently;
B. heating the beaker treated in the step A to 80-90 ℃, stirring at a constant temperature for 8-12min, then sequentially adding the aluminum sulfate, the starch, the defoaming agent and the preservative prepared in the step 1) into the beaker, stirring for 3-5min, cooling to room temperature after stirring, forming a bonding layer on the surface of the glass substrate, and taking out the glass substrate for later use; in the step B, raw materials such as aluminum sulfate and the like are added into a beaker, and the produced polyvinyl alcohol reacts with the raw materials to form a bonding layer on the surface of the antireflection film;
c) coating of the modified silica gel layer:
A. putting the tetraethyl silicate and the ethanol prepared in the step 1) into a beaker, performing magnetic stirring at room temperature, slowly dropwise adding the ammonia water prepared in the step 1) into the beaker in the stirring process, and continuing stirring for 250-260min after dropwise adding the ammonia water; standing and aging for 10-12h to obtain silicon dioxide gel;
B. diluting the heptadecafluorodecyltrimethoxysilane and the gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane prepared in the step 1) with ethanol, sequentially adding into the beaker in the step A, and ultrasonically stirring for 1-2h to obtain modified silica gel; b, preparing modified silica gel;
C. placing the glass substrate treated in the step a) on a spin coating platform, enabling one side of the glass substrate which is not coated with the masking film to face downwards, and uniformly dropwise adding the modified silica gel prepared in the step B, wherein the spin coating is carried out for 1-2min, and the rotating speed is 1400-1600 rpm; then placing on a hot plate and heating for 2-4min, wherein the temperature of the hot plate is 90-110 ℃; repeatedly throwing the gel for 3-5 times, and then putting the gel into an oven for thermosetting to form a modified silicon dioxide gel layer; wherein the thermosetting temperature is 90-100 ℃, and the thermosetting time is 30-40 min; in the step C, the prepared modified silica gel is uniformly coated on the bonding layer in a spin coating and whirl coating mode, the agglomerated silica particles can form a multi-layer micro-nano hole structure, when water drops contact with the surface of the coated glass, the multi-layer hole structure can enable the surface to form an air film, the contact area of the liquid drops and the surface of the coated glass is reduced, and therefore the super-hydrophobic performance of the coated glass is achieved;
5) removing the masking film: taking the glass substrate treated in the step 4), removing the masking film on one side of the glass substrate, and then washing for 2-4 times by using deionized water; removing the mask film in the step 5);
6) and finishing the operation.
Preferably, in the step 2), the temperature for low-temperature curing is 280-300 ℃, and the curing time is 2-5 min.
Preferably, in the step c) of the step 1), when the glass substrate is cleaned, the cut glass substrate is taken and put into a sodium hydroxide solution for soaking for 20-30min, and then is washed by deionized water and dried by nitrogen for standby.
Compared with the prior art, the invention has the beneficial effects that:
when the method is operated, firstly, the raw materials are prepared, the glass substrate is cleaned, and oil stains on the surface of the glass substrate are removed and the surface of the glass substrate is kept dry; coating an antireflection film on one side of the glass substrate, and coating a masking film on the other side of the glass substrate, wherein the masking film can play a role in protection, so that the situation that when a self-cleaning coating is coated, the self-cleaning coating is also coated on the side, which does not need to be processed, of the glass substrate is avoided; then, the bonding layer is generated while the rough surface is formed on the antireflection film, so that the bonding layer can be smoothly and tightly combined with the antireflection film; and then, preparing modified silica gel, coating the modified silica gel on the bonding layer to form a modified silica gel layer, wherein the modified silica gel layer is used as a super-hydrophobic surface, and the super-hydrophobic property and the self-cleaning property of the coated glass can be effectively improved.
The technical scheme discloses coated glass with a self-cleaning surface and a preparation method thereof, the process is reasonable in design and simple to operate, the bonding performance between a self-cleaning coating and an antireflection film is effectively improved, the service life of the coated glass is prolonged, and meanwhile, a super-hydrophobic plane is formed on the surface of the coated glass by modifying silicon dioxide gel, so that the super-hydrophobic performance and the self-cleaning performance of the coated glass are effectively improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
step S1: preparing raw materials; weighing tetraethyl silicate, ethanol, ammonia water, heptadecafluorodecyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane according to a proportion for later use; weighing methanol, vinyl acetate, sodium hydroxide, aluminum sulfate, a defoaming agent, a preservative and starch according to a proportion for later use;
step S2: cleaning a glass substrate, wherein when the glass substrate is cleaned, the cut glass substrate is taken and put into a sodium hydroxide solution for soaking for 20min, then is washed by deionized water, and is dried by nitrogen for standby;
step S3: coating of an antireflection film: coating an antireflection film liquid on the surface of one side of the glass substrate by using a roll coating method, and curing at a low temperature to form an antireflection film; the low-temperature curing temperature is 280 ℃, and the curing time is 5 min;
step S4: coating a layer of photoresist on one side of the treated glass substrate which is not coated with the antireflection film, and baking to solidify the shielding film to form a shielding film; wherein the baking temperature is 95 ℃, and the baking time is 20 min;
step S5: coating of the self-cleaning coating:
step S51: preparing polyvinyl alcohol, namely putting prepared methanol into a four-neck flask provided with a stirrer, a condenser pipe, a thermometer and a dropping funnel, adding a sodium hydroxide solution, starting the stirrer to stir for 2 min; then placing the prepared vinyl acetate into a dropping funnel, slowly dropping the prepared vinyl acetate into a four-neck flask within 25min, and stirring for reacting for 1.5h to obtain a first material;
step S52: coating of the bonding layer: pouring the first material after the reaction is finished into a beaker, putting the glass substrate treated in the step 3) into the beaker, heating to 40 ℃, and reacting for 25 min; heating the beaker to 80 ℃, stirring at a constant temperature for 12min, sequentially adding the prepared aluminum sulfate, starch, defoaming agent and preservative into the beaker, stirring for 3min, cooling to room temperature after stirring, forming a bonding layer on the surface of the glass substrate, and taking out the glass substrate for later use;
step S6: coating of the modified silica gel layer: putting the prepared tetraethyl silicate and ethanol into a beaker, performing magnetic stirring at room temperature, slowly dropwise adding the prepared ammonia water into the beaker in the stirring process, and continuously stirring for 250min after dropwise adding of the ammonia water is finished; standing and aging for 10h to obtain silicon dioxide gel; diluting the prepared heptadecafluorodecyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane with ethanol, sequentially putting into a beaker, and ultrasonically stirring for 1h to obtain modified silica gel;
placing the glass substrate treated in the step S5 on a whirl coating platform, enabling the side, which is not coated with the masking film, to face downwards, uniformly and dropwise adding modified silica gel, wherein whirl coating is carried out for 1min, and the rotating speed is 1400 rpm; then placing on a hot plate and heating for 2min, wherein the temperature of the hot plate is 110 ℃; repeatedly throwing the gel for 3 times, and then putting the gel into an oven for thermosetting to form a modified silicon dioxide gel layer; wherein the thermosetting temperature is 90 ℃ and the thermosetting time is 40 min;
step S7: removing the masking film: taking the treated glass substrate, removing the masking film on one side of the glass substrate, and then cleaning for 2 times by using deionized water; and finishing the operation.
In the embodiment, the thickness of the antireflection film is 50nm, and the thickness of the self-cleaning coating is 100 nm; the thickness of the bonding layer is 50nm, and the thickness of the modified silicon dioxide gel layer is 50 nm.
Wherein the modified silica gel layer comprises the following raw material components: by weight, 15 parts of tetraethyl silicate, 10 parts of ethanol, 20 parts of ammonia water, 5 parts of heptadecafluorodecyltrimethoxysilane and 3 parts of a crosslinking agent; the bonding layer comprises the following raw material components: by weight, 8 parts of methanol, 15 parts of vinyl acetate, 5 parts of sodium hydroxide, 5 parts of aluminum sulfate, 3 parts of a defoaming agent, 3 parts of a preservative and 2 parts of starch; the cross-linking agent is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane.
Example 2:
step S1: preparing raw materials; weighing tetraethyl silicate, ethanol, ammonia water, heptadecafluorodecyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane according to a proportion for later use; weighing methanol, vinyl acetate, sodium hydroxide, aluminum sulfate, a defoaming agent, a preservative and starch according to a proportion for later use;
step S2: cleaning a glass substrate, wherein when the glass substrate is cleaned, the cut glass substrate is taken and put into a sodium hydroxide solution for soaking for 25min, then is washed by deionized water, and is dried by nitrogen for standby;
step S3: coating of an antireflection film: coating an antireflection film liquid on the surface of one side of the glass substrate by using a roll coating method, and curing at a low temperature to form an antireflection film; the temperature for low-temperature curing is 290 ℃, and the curing time is 4 min;
step S4: coating a layer of photoresist on one side of the treated glass substrate which is not coated with the antireflection film, and baking to solidify the shielding film to form a shielding film; wherein the baking temperature is 98 ℃, and the baking time is 18 min;
step S5: coating of the self-cleaning coating:
step S51: preparing polyvinyl alcohol, namely putting prepared methanol into a four-neck flask provided with a stirrer, a condenser pipe, a thermometer and a dropping funnel, adding a sodium hydroxide solution, starting the stirrer to stir for 4 min; then placing the prepared vinyl acetate into a dropping funnel, slowly dropping the prepared vinyl acetate into a four-neck flask within 30min, and stirring for reacting for 2h to obtain a first material;
step S52: coating of the bonding layer: pouring the first material after the reaction is finished into a beaker, putting the glass substrate treated in the step 3) into the beaker, heating to 45 ℃, and reacting for 20 min; heating the beaker to 85 ℃, stirring at a constant temperature for 10min, sequentially adding the prepared aluminum sulfate, starch, defoaming agent and preservative into the beaker, stirring for 4min, cooling to room temperature after stirring, forming a bonding layer on the surface of the glass substrate, and taking out the glass substrate for later use;
step S6: coating of the modified silica gel layer: putting the prepared tetraethyl silicate and ethanol into a beaker, performing magnetic stirring at room temperature, slowly dropwise adding the prepared ammonia water into the beaker in the stirring process, and continuously stirring for 255min after dropwise adding of the ammonia water is finished; standing and aging for 11h to obtain silicon dioxide gel; diluting the prepared heptadecafluorodecyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane with ethanol, sequentially putting into a beaker, and ultrasonically stirring for 1.5h to obtain modified silica gel;
placing the glass substrate treated in the step S5 on a whirl coating platform, enabling the side, which is not coated with the masking film, to face downwards, uniformly and dropwise adding modified silica gel, wherein whirl coating is performed for 1.5min, and the rotating speed is 1500 rpm; then placing on a hot plate and heating for 3min, wherein the temperature of the hot plate is 100 ℃; repeatedly throwing the gel for 4 times, and then putting the gel into an oven for thermosetting to form a modified silicon dioxide gel layer; wherein the thermosetting temperature is 95 ℃, and the thermosetting time is 35 min;
step S7: removing the masking film: taking the treated glass substrate, removing the masking film on one side of the glass substrate, and then cleaning for 3 times by using deionized water; and finishing the operation.
In the embodiment, the thickness of the antireflection film is 80nm, and the thickness of the self-cleaning coating is 160 nm; the thickness of the bonding layer is 80nm, and the thickness of the modified silicon dioxide gel layer is 80 nm.
Wherein the modified silica gel layer comprises the following raw material components: by weight, 20 parts of tetraethyl silicate, 15 parts of ethanol, 30 parts of ammonia water, 10 parts of heptadecafluorodecyltrimethoxysilane and 5 parts of a cross-linking agent; the bonding layer comprises the following raw material components: by weight, 12 parts of methanol, 24 parts of vinyl acetate, 8 parts of sodium hydroxide, 9 parts of aluminum sulfate, 4 parts of a defoaming agent, 4 parts of a preservative and 4 parts of starch; the cross-linking agent is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane.
Example 3:
step S1: preparing raw materials; weighing tetraethyl silicate, ethanol, ammonia water, heptadecafluorodecyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane according to a proportion for later use; weighing methanol, vinyl acetate, sodium hydroxide, aluminum sulfate, a defoaming agent, a preservative and starch according to a proportion for later use;
step S2: cleaning a glass substrate, wherein when the glass substrate is cleaned, the cut glass substrate is taken and put into a sodium hydroxide solution for soaking for 30min, then is washed by deionized water, and is dried by nitrogen for standby;
step S3: coating of an antireflection film: coating an antireflection film liquid on the surface of one side of the glass substrate by using a roll coating method, and curing at a low temperature to form an antireflection film; the temperature for low-temperature curing is 300 ℃, and the curing time is 2 min;
step S4: coating a layer of photoresist on one side of the treated glass substrate which is not coated with the antireflection film, and baking to solidify the shielding film to form a shielding film; wherein the baking temperature is 100 ℃, and the baking time is 15 min;
step S5: coating of the self-cleaning coating:
step S51: preparing polyvinyl alcohol, namely putting prepared methanol into a four-neck flask provided with a stirrer, a condenser pipe, a thermometer and a dropping funnel, adding a sodium hydroxide solution, starting the stirrer to stir for 5 min; then placing the prepared vinyl acetate into a dropping funnel, slowly dropping the prepared vinyl acetate into a four-neck flask within 35min, and stirring for reacting for 2.5h to obtain a first material;
step S52: coating of the bonding layer: pouring the first material after the reaction is finished into a beaker, putting the glass substrate treated in the step 3) into the beaker, heating to 50 ℃, and reacting for 15 min; heating the beaker to 90 ℃, stirring at a constant temperature for 8min, sequentially adding the prepared aluminum sulfate, starch, defoaming agent and preservative into the beaker, stirring for 5min, cooling to room temperature after stirring, forming a bonding layer on the surface of the glass substrate, and taking out the glass substrate for later use;
step S6: coating of the modified silica gel layer: putting the prepared tetraethyl silicate and ethanol into a beaker, performing magnetic stirring at room temperature, slowly dropwise adding the prepared ammonia water into the beaker in the stirring process, and continuously stirring for 260min after dropwise adding of the ammonia water is finished; standing and aging for 12h to obtain silicon dioxide gel; diluting the prepared heptadecafluorodecyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane with ethanol, sequentially putting into a beaker, and ultrasonically stirring for 2h to obtain modified silica gel;
placing the glass substrate treated in the step S5 on a whirl coating platform, enabling the side, which is not coated with the masking film, to face downwards, uniformly and dropwise adding modified silica gel, and whirl coating for 2min at the rotating speed of 1600 rpm; then placing on a hot plate and heating for 4min, wherein the temperature of the hot plate is 90 ℃; repeatedly throwing the gel for 5 times, and then putting the gel into an oven for thermosetting to form a modified silicon dioxide gel layer; wherein the thermosetting temperature is 100 ℃, and the thermosetting time is 30 min;
step S7: removing the masking film: taking the treated glass substrate, removing the masking film on one side of the glass substrate, and then cleaning for 4 times by using deionized water; and finishing the operation.
In the embodiment, the thickness of the antireflection film is 100nm, and the thickness of the self-cleaning coating is 200 nm; the thickness of the bonding layer is 100nm, and the thickness of the modified silicon dioxide gel layer is 100 nm.
Wherein the modified silica gel layer comprises the following raw material components: by weight, 25 parts of tetraethyl silicate, 20 parts of ethanol, 40 parts of ammonia water, 15 parts of heptadecafluorodecyltrimethoxysilane and 8 parts of a cross-linking agent; the bonding layer comprises the following raw material components: 16 parts of methanol, 30 parts of vinyl acetate, 10 parts of sodium hydroxide, 12 parts of aluminum sulfate, 5 parts of a defoaming agent, 6 parts of a preservative and 6 parts of starch by weight; the cross-linking agent is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane.
Experiment 1:
taking the coated glass samples prepared in the examples 1 to 3, taking the self-cleaning coated glass purchased from the market, and detecting the water contact angle of the coated glass: the contact angle of the invention adopts a sessile drop contact angle tester to test the wetting angle of a water drop on the surface of self-cleaning glass, the contact angles of 5 different positions on the surface of a film are measured, and the average value of the contact angles is taken as the surface contact angle of the film, and the result of the invention is as follows:
after the samples in the examples 1 to 3 are detected, the water contact angles of the glass surface are 155 degrees, 157 degrees and 151 degrees respectively; and the surface water contact angle of the commercially available coated glass is 132 degrees.
And (4) conclusion: the technical scheme discloses coated glass with a self-cleaning surface and a preparation method thereof.
Experiment 2: the film adhesion of each of the self-cleaning glasses of examples 1 to 3 and commercially available ones was tested, and the results were as follows:
the samples of examples 1-3 were tested to show 25N, 28N, and 23N adhesion, respectively, whereas commercially available coated glass showed 11N adhesion.
And (4) conclusion: according to the technical scheme, the bonding layer is generated while the rough surface is formed on the antireflection film, so that the bonding layer can be smoothly and tightly combined with the antireflection film, and the tight combination of the antireflection film and the modified silicon dioxide gel layer is effectively improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (1)
1. A coated glass with a self-cleaning surface is characterized in that: the coated glass comprises a glass substrate, an antireflection film and a self-cleaning coating, wherein the antireflection film is coated on the surface of one side of the glass substrate, and the self-cleaning coating is coated on the antireflection film; the self-cleaning coating comprises an adhesive layer and a modified silicon dioxide gel layer, wherein the adhesive layer is coated on the antireflection film, and the modified silicon dioxide gel layer is coated on the adhesive layer;
the preparation method of the coated glass comprises the following steps:
step S1: preparing raw materials; weighing tetraethyl silicate, ethanol, ammonia water, heptadecafluorodecyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane according to a proportion for later use; weighing methanol, vinyl acetate, sodium hydroxide, aluminum sulfate, a defoaming agent, a preservative and starch according to a proportion for later use;
step S2: cleaning a glass substrate, wherein when the glass substrate is cleaned, the cut glass substrate is taken and put into a sodium hydroxide solution for soaking for 25min, then is washed by deionized water, and is dried by nitrogen for standby;
step S3: coating of an antireflection film: coating an antireflection film liquid on the surface of one side of the glass substrate by using a roll coating method, and curing at a low temperature to form an antireflection film; the temperature for low-temperature curing is 290 ℃, and the curing time is 4 min;
step S4: coating a layer of photoresist on one side of the treated glass substrate which is not coated with the antireflection film, and baking to solidify the shielding film to form a shielding film; wherein the baking temperature is 98 ℃, and the baking time is 18 min;
step S5: coating of the self-cleaning coating:
step S51: preparing polyvinyl alcohol, namely putting prepared methanol into a four-neck flask provided with a stirrer, a condenser pipe, a thermometer and a dropping funnel, adding a sodium hydroxide solution, starting the stirrer to stir for 4 min; then placing the prepared vinyl acetate into a dropping funnel, slowly dropping the prepared vinyl acetate into a four-neck flask within 30min, and stirring for reacting for 2h to obtain a first material;
step S52: coating of the bonding layer: pouring the first material after the reaction is finished into a beaker, putting the glass substrate treated in the step 3) into the beaker, heating to 45 ℃, and reacting for 20 min; heating the beaker to 85 ℃, stirring at a constant temperature for 10min, sequentially adding the prepared aluminum sulfate, starch, defoaming agent and preservative into the beaker, stirring for 4min, cooling to room temperature after stirring, forming a bonding layer on the surface of the glass substrate, and taking out the glass substrate for later use;
step S6: coating of the modified silica gel layer: putting the prepared tetraethyl silicate and ethanol into a beaker, performing magnetic stirring at room temperature, slowly dropwise adding the prepared ammonia water into the beaker in the stirring process, and continuously stirring for 255min after dropwise adding of the ammonia water is finished; standing and aging for 11h to obtain silicon dioxide gel; diluting the prepared heptadecafluorodecyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane with ethanol, sequentially putting into a beaker, and ultrasonically stirring for 1.5h to obtain modified silica gel;
placing the glass substrate treated in the step S5 on a whirl coating platform, enabling the side, which is not coated with the masking film, to face downwards, uniformly and dropwise adding modified silica gel, wherein whirl coating is performed for 1.5min, and the rotating speed is 1500 rpm; then placing on a hot plate and heating for 3min, wherein the temperature of the hot plate is 100 ℃; repeatedly throwing the gel for 4 times, and then putting the gel into an oven for thermosetting to form a modified silicon dioxide gel layer; wherein the thermosetting temperature is 95 ℃, and the thermosetting time is 35 min;
step S7: removing the masking film: taking the treated glass substrate, removing the masking film on one side of the glass substrate, and then cleaning for 3 times by using deionized water; finishing the operation;
the thickness of the antireflection film is 80nm, and the thickness of the self-cleaning coating is 160 nm; the thickness of the bonding layer is 80nm, and the thickness of the modified silicon dioxide gel layer is 80 nm;
the modified silica gel layer comprises the following raw material components: by weight, 20 parts of tetraethyl silicate, 15 parts of ethanol, 30 parts of ammonia water, 10 parts of heptadecafluorodecyltrimethoxysilane and 5 parts of a cross-linking agent; the bonding layer comprises the following raw material components: by weight, 12 parts of methanol, 24 parts of vinyl acetate, 8 parts of sodium hydroxide, 9 parts of aluminum sulfate, 4 parts of a defoaming agent, 4 parts of a preservative and 4 parts of starch; the cross-linking agent is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane.
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| CN113045216A (en) * | 2021-03-02 | 2021-06-29 | 胡敏文 | Self-cleaning coated glass for curtain wall and preparation method thereof |
| CN117003492A (en) * | 2023-08-07 | 2023-11-07 | 厦门晶晟能源科技有限公司 | Vacuum low-radiation power generation glass for photovoltaic building integration |
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| CN114315166A (en) * | 2021-12-17 | 2022-04-12 | 常州龙腾光热科技股份有限公司 | Glass sleeve coating structure of vacuum heat collecting tube and preparation method thereof |
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| CN110451819B (en) | 2020-08-07 |
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