CN105754381B - A kind of nanometer anti-reflection coating liquid and its preparation method and application - Google Patents
A kind of nanometer anti-reflection coating liquid and its preparation method and application Download PDFInfo
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- CN105754381B CN105754381B CN201510096555.5A CN201510096555A CN105754381B CN 105754381 B CN105754381 B CN 105754381B CN 201510096555 A CN201510096555 A CN 201510096555A CN 105754381 B CN105754381 B CN 105754381B
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- 239000007788 liquid Substances 0.000 title claims abstract description 82
- 238000000576 coating method Methods 0.000 title claims abstract description 79
- 239000011248 coating agent Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002105 nanoparticle Substances 0.000 claims abstract description 29
- 239000002318 adhesion promoter Substances 0.000 claims abstract description 24
- 239000004088 foaming agent Substances 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 235000019441 ethanol Nutrition 0.000 claims description 20
- 239000000080 wetting agent Substances 0.000 claims description 19
- 239000002270 dispersing agent Substances 0.000 claims description 18
- 239000006185 dispersion Substances 0.000 claims description 18
- 238000007761 roller coating Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 8
- 239000007822 coupling agent Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- -1 zirconium ester Chemical class 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 239000001023 inorganic pigment Substances 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 150000007942 carboxylates Chemical class 0.000 claims description 2
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 2
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000005543 nano-size silicon particle Substances 0.000 claims description 2
- 239000002736 nonionic surfactant Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims 2
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- XNSIKGLUWHSURK-UHFFFAOYSA-N C(CC)[Si](OCC)(OCC)OCC.[O] Chemical compound C(CC)[Si](OCC)(OCC)OCC.[O] XNSIKGLUWHSURK-UHFFFAOYSA-N 0.000 claims 1
- 150000004645 aluminates Chemical class 0.000 claims 1
- 229920001577 copolymer Polymers 0.000 claims 1
- 238000003618 dip coating Methods 0.000 claims 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 235000011187 glycerol Nutrition 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- 238000010276 construction Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 54
- 239000011521 glass Substances 0.000 description 41
- 238000002834 transmittance Methods 0.000 description 15
- 239000010410 layer Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 13
- 238000003756 stirring Methods 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 6
- 239000002103 nanocoating Substances 0.000 description 6
- 239000004576 sand Substances 0.000 description 6
- 239000007888 film coating Substances 0.000 description 5
- 238000009501 film coating Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000012780 transparent material Substances 0.000 description 5
- 238000009739 binding Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 230000002269 spontaneous effect Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000012267 brine Substances 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 229910002013 Aerosil® 90 Inorganic materials 0.000 description 1
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000003667 anti-reflective effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000011514 reflex Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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- Paints Or Removers (AREA)
Abstract
The invention discloses a kind of nanometer anti-reflection coating liquids and its preparation method and application.The nanometer anti-reflection coating liquid, formula includes following components in parts by weight：0.1~5 part of nano particle, 0.1~20 part of pore-foaming agent, 0.1~5 part of adhesion promoter, 0.01~10 part of auxiliary agent, 80~99 parts of solvent.The present invention obtains nanometer anti-reflection coating liquid first by nano particle grinding distribution in the solvent dissolved with adhesion promoter and auxiliary agent, then by itself and pore-foaming agent and auxiliary agent etc. are compound.The coating liquid may be used a variety of construction coating process and be coated on different transparent substrate surfaces, and anti-reflection coating is formed in substrate surface after high-temperature baking.
Description
Technical field
The present invention relates to chemical industry, nano material, film preparation and clean energy resource field more particularly to a kind of nanometer anti-reflections
Coating liquid and its preparation method and application.
Background technology
Now, transparent material is widely used in industry-by-industry, such as solar cell cover-plate glass, optical device.By
In refraction index difference, light still can generate reflex when passing through transparent material in air/material interface, thus cannot
It all penetrates, reduces its light transmittance.For example, glass is most commonly seen transparent material, the single face reflectivity of simple glass
About 4%, therefore its total light transmittance is difficult more than 92%.For the more demanding system of some transparencys, such as solar-electricity
For pond, display screen and optical device etc., the 8% visible light proportion of goods damageds can largely effect on the energy ecology of equipment.With
For solar cell, if the visible light transmittance of glass can further increase, the energy conversion efficiency of solar cell
It can then greatly improve.And for display screen material, the raising of screen glass light transmittance can then be reduced to the bright of backboard
Degree requires, and to which the power consumption of equipment be greatly reduced, extends the service life of battery.
In general, the film by preparing one or more layers low refractive index in substrate surface, reduces light at interface
Reflectivity, the light penetration of material can be improved.Still by taking glass as an example, the refraction index of glass is about 1.5, theory meter
It obtains, if forming the film that one layer of refraction index is 1.25 in glass surface, the light transmittance of glass can be increased to
100%.But the refraction index for the material (magnesium fluoride) that refraction index known to nature is minimum is also only 1.38.Therefore, mesh
Preceding is mainly by introducing hole in film layer, the refraction index of film being reduced using the low refractive index (1.0) of air.
From the point of view of technological angle, the preparation method of anti-reflection film includes mainly following several：Etching method, vacuum vapour deposition and
Sol-gel method.Etching method performs etching Inorganic Substrate Surface layer generally by the substance of strong corrosive, to reduce
The consistency of glass surface forms the anti-reflection thin layer of high porosity.CN102674704 and CN102491649 is utilized respectively fluorine-containing
Strong acid and disodium hydrogen phosphate/aluminium chloride mixed liquor glass is performed etching and has obtained porous antireflection layer in glass surface.It should
The defect of method is that flow is longer, and the etchant used is high, not environmentally, there is security risk.Vacuum Coating method includes
Magnetron sputtering and vapour deposition process etc., common feature are under vacuum conditions, by the gasification of high-purity target target or ion
Physics or chemical reaction occur again for change, and thin layer is generated in substrate surface.Exist as magnetron sputtering technique is utilized in CN20244455
Glass surface is prepared for the anti-reflection coating with multi-layer film structure.Vacuum Coating method can prepare highly uniform anti-reflection of film thickness
Layer, but process conditions are very harsh, equipment cost is higher.
In comparison, the filming equipment of sol-gel method is simple, can be operated under normal temperature and pressure conditions, and technical recipe
Modulatory character it is high, therefore application is more extensive.The technique is using the compound containing high chemical active ingredient as presoma, by it
Be mixed to get clear solution with alcohols or ketones solvent, add suitable water cause hydrolysis-condensation reaction obtain it is transparent molten
It is then coated on substrate surface, is heat-treated after its drying and forming-film, then can obtain inorganic anti-reflection film by glue.Subsequently
The main function of heat treatment process is to be sintered solidification to the gel layer formed in drying and forming-film process to obtain containing hole
Antireflection layer.CN103524049 discloses a kind of preparation method of single layer antireflecting silicon dioxide film.This method is first by silica
Organic precursor is dissolved in acid alcohol/water mixed liquid, then after it after substrate glass surface filming, using 200~400 DEG C
It is thermally treated resulting in single layer silica plated film.For another example CN102850894 is first prepared for the different complex sol of size, then by its with
Coalescents are blended in substrate surface and prepare anti-reflection coating.Although the method is simple, lacking for its large-scale industrial application is influenced
Point is that the storage stability of colloidal sol is poor, because most of colloidal sols are thermodynamically in metastable state, is being stored so as to cause it
Flocculation or sedimentation can be generated due to uncontrollable hydrolysis-condensation reaction after a certain period of time.
So if anti-reflection film coating liquid can be prepared from stable nano particle, then technique and product can be greatly improved
Stability.However currently without the anti-reflection membrane preparation method based on nano particle of comparative maturity, be primarily due to compared to
Sol-gel method prepares coating liquid from particle directness, to the more demanding of plated film formula of liquid and technique.CN102795791
Although being prepared for anti-reflection film by raw material of nanometer silicon dioxide particle, acted on layer by layer using based on electrostatic attraction
Self-assembly process.The technological process is complicated, while to the extremely low (grain amount lost during actual process of the utilization ratio of raw material
For the several times or even decades of times of the grain amount of actual participation film forming), so not utilizing extensive commercial application.In addition, particle
Film is needed in application other problem solved is that adhesive force is inadequate between film layer and base material, this leverages it and uses the longevity
Life.
Invention content
Technical problem to be solved by the present invention lies in overcome existing thin film fabrication techniques route complex process, cost compared with
High, the defects of service life is short, a kind of nanometer anti-reflection coating liquid is provided, and the transparent of anti-reflection film is coated with made from it
Base material.
The present invention from nano particle, can by be formulated design and processes optimization prepare it is stable, there is anti-reflection work(
The coating liquid of energy.The coating liquid can form plated film with base material binding force jail, with high anti-reflection rate in substrate surface.This hair
It is bright by introducing pore-foaming agent in formula so that plated film forms spontaneous hole during high-temperature baking.Compared to by natural packing
The hole of formation, spontaneous pore size is smaller, more uniformly, therefore can assign the higher anti-reflection rate of anti-reflection coating of gained.This
Outside, the present invention also adds adhesion promoter in formula, can be reacted with the active group (such as hydroxyl) of substrate surface
Bonding, so as to improve the adhesive force between plated film and base material.Compared to existing coating technique, nanometer proposed by the present invention
Anti-reflection film coating liquid preparation process flow is simple, and coating liquid stability is high, and coating process mild condition has wide range of applications, and can
To use a variety of different coating process.
The present invention provides a kind of nanometer anti-reflection coating liquid, composition of raw materials includes following components in parts by weight：It receives
0.1~5 part of rice grain, 0.1~20 part of pore-foaming agent, 0.1~5 part of adhesion promoter, 0.01~10 part of auxiliary agent, solvent 80~99
Part.
Wherein, the solid content of the nanometer anti-reflection coating liquid is 1~30%.The nano particle is nano metal oxygen
Compound, nano metal fluoride and nano nonmetal oxide, including nano silicon dioxide, nano-titanium dioxide, nanometer fluorine
Change one or more of the compound of magnesium, nano aluminium oxide and above-mentioned nano particle.Its initial size is 5 nanometers~150
Nanometer.The nano particle used in the more preferable embodiment of the present invention of the nano particle.
Wherein, thermal weight loss can occur when being heated to 300 DEG C or more for the pore-foaming agent, be polyvinylpyrrolidone,
Polynary acid polymer, polyethylene oxide (PEG), polypropylene oxide (PPG), ethylene oxide/propylene oxide (block) copolymer, hydroxyl
One or more of propyl cellulose, polymethylacrylic acid (ester), polyacrylic acid (ester), polyurethane or silicones.Described
The pore-foaming agent used in the more preferable embodiment of the present invention of pore-foaming agent.
Wherein, the adhesion promoter is silane coupling agent, titanate coupling agent, zirconium ester coupling agent and aluminic acid
One or more of zirconium coupling agent；Preferably 3-aminopropyltriethoxysilane, 3- TSL 8330s,
γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-glycidoxypropyltrietandysilane andysilane, γ-methacryl
It is one or more in base trimethoxy silane and γ-methacryloxypropyl described in oxygroup third；
And/or the dosage of the adhesion promoter accounts for the 5~150% of the nanoparticle weight.The adhesive force promotes
The adhesion promoter used in the more preferable embodiment of the present invention of agent.
Wherein, the auxiliary agent is one or more in dispersant and wetting agent.The molecule knot of the dispersant
Structure should include simultaneously：The group to inorganic pigment with affinity, such as carboxyl, carboxylate, phosphate-based, amino, ammonium root, polynary
Amine, polyacid and polyethers；The macromolecular chain being easily completely solvated, such as polyester, polyethers and polyacrylate；And/or it is described
The dosage of dispersant accounts for the 15~150% of the nanoparticle weight.The wetting agent should can reduce the table of coating liquid
It is one or more in face tension, preferably organosilicon compound, fluorocarbons and nonionic surfactant；
And/or the dosage of the wetting agent accounts for the 0~20% of the nanoparticle weight.The dispersant more preferably this hair
The dispersant used in bright embodiment, the wetting agent used in the more preferable embodiment of the present invention of the wetting agent.
Wherein, the solvent is water, ethyl alcohol, isopropanol, n-butanol, ethylene glycol, propylene glycol, acetone, 2- butanone, acetic acid
It is one or more in ethyl ester, butyl acetate and dimethylbenzene；
Wherein, the preparation flow of the nanometer anti-reflection coating liquid includes two basic steps：
(1) adhesion promoter and auxiliary agent (preferably dispersant) are dissolved in solvent, add nano particle, to its into
Row ultrasound, then ball milling or sanded treatment, obtain dispersion liquid；
(2) pore-foaming agent is dissolved in solvent, then under agitation, sequentially adds the dispersion liquid obtained by step (1) and helped
Agent (preferably wetting agent), after mixing, you can obtain nanometer anti-reflection coating liquid.
The present invention also provides a kind of transparent bases being coated with anti-reflection film, are worth by following methods：Using showering, leaching
Apply, the method for spraying or roller coating by the nanometer anti-reflection coating liquid even application on the surface of transparent material, then 300~
It is toasted 1~10 minute under the conditions of 900 DEG C, you can anti-reflection coating is made in transparent material surface.The transparent base can be used
Various conventional transparent bases, such as glass.
On the basis of common knowledge of the art, above-mentioned each optimum condition can be combined arbitrarily to get each preferable reality of the present invention
Example.
The reagents and materials used in the present invention are commercially available.
The positive effect of the present invention is that：
Compared with prior art, the present invention designs and prepares technique by the formula of optimization, by initial size 5~150
The nano particle of nanometer is successfully combined with each other with other functional materials such as pore-foaming agent and adhesion promoter, is had
There is the nano-coating liquid of excellent anti-reflection function.The pore-foaming agent that the coating liquid uses when being toasted at 300 DEG C or more can in plated film shape
At spontaneous hole, the index of refraction of plated film can be greatly reduced, improve the visible light transmittance of base material, to realize anti-reflection effect
Fruit.Meanwhile the coating liquid also uses the adhesion promoter of coupling agent class, it can be with functional group (such as hydroxyl of substrate surface
Base) binding reaction, the binding force that can be obviously improved between plated film and base material, to extend the service life of plated film occurs.
The coating liquid may be used a variety of different construction means and form a film in different transparent substrate surfaces.By taking glass as an example, the coating liquid
After vitreous coating by high-temperature baking can fast filming, enormously simplify coating process, and improve the stability of technique,
Therefore the large-scale industrialized production of anti-reflection film coating liquid and the material containing anti-reflection coating can be realized.
Description of the drawings
Fig. 1 is the transmission electron microscopy observation result for the dispersion liquid that embodiment 1 obtains.
Specific implementation mode
It is further illustrated the present invention below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
Product specification selects.
Embodiment 1 has the alcohol system nano-coating liquid I of anti-reflection function
The formula of alcohol system nano-coating liquid I with anti-reflection function see the table below：
Preparation method：
Dispersant and adhesion promoter are first dissolved in ethyl alcohol, nano particle is added under agitation, is uniformly mixed
Afterwards, it is ground 3 hours in sand mill, obtains stable dispersion liquid.Its particle deployment conditions is by transmission electron microscope (TEM) table
Sign, as shown in Figure 1.Tem observation the result shows that, nanometer silicon dioxide particle is uniformly divided in the dispersion liquid of gained with reset condition
It dissipates in solvent, no apparent aggregate exists.
Pore-foaming agent is dissolved in ethyl alcohol, then above-mentioned dispersion liquid and wetting agent is added in stirring condition successively, is stirred
Alcohol system nanometer anti-reflection coating liquid is obtained after even.
The nanometer anti-reflection plated film of 2 different-thickness of embodiment
Preparation method：By the nanometer anti-reflection coating liquid roller coating of 1 gained of embodiment in glass surface, by controlling roller coating speed
Degree, by 600 DEG C, baking in 2 minutes, glass surface formed film thickness be respectively 140 nanometers~150 nanometers, 150 nanometers~
170 nanometers and 180 nanometers~200 nanometers of anti-reflection coating.
The anti-reflection performance of gained plated film by desk-top transmittance spectroscopic measurements instrument, (test by the desk-top spectral transmittance of extensive and profound in meaning Thailand's air supporting
System (model Filmeasure 2100) characterizes.Test result is as follows for gained shown in table：
The result shows that the coated glass of gained is above non-coated glass in the light transmittance of visible region, and anti-reflection peak pair
The position answered and film thickness are closely related.
When film thickness is 140-150 nanometers, gained coated glass is high in 560 nanometers to 600 nano wave length sections of light transmittance
Up to 94.7%, compared to the light transmittance of commonly non-coated glass 92%, anti-reflection rate reaches 2.7%.
When film thickness is 150-170 nanometers, gained coated glass is high in 600 nanometers to 680 nano wave length sections of light transmittance
Up to 95.0%, compared to the light transmittance of commonly non-coated glass 92%, anti-reflection rate reaches 3.0%.
When film thickness is 180-200 nanometers, gained coated glass is high in 720 nanometers to 800 nano wave length sections of light transmittance
Up to 93.5%, compared to the light transmittance of commonly non-coated glass 92%, anti-reflection rate reaches 2.3%.
3 water-based system nanometer anti-reflection coating liquid of embodiment and anti-reflection coating
The formula of water nano anti-reflection film coating liquid with anti-reflection function see the table below：
Preparation method：
Dispersant and adhesion promoter are first dissolved in water, nano particle is added under agitation, after mixing,
It is ground 8 hours in sand mill, obtains stable dispersion liquid.
Pore-foaming agent is soluble in water, then above-mentioned dispersion liquid and wetting agent is added in stirring condition successively, it is uniformly mixed
Obtain water nano anti-reflection film coating liquid afterwards.
By the nanometer anti-reflection coating liquid roller coating of gained in glass surface, by controlling roll coating speeds, by 700 DEG C, 5 minutes
Baking, it is respectively 150 nanometers~170 nanometers of anti-reflection coating to form film thickness in glass surface.The light transmission of gained anti-reflection film
Rate is higher than non-coated glass by 2.6%.
4 solvent type nanometer anti-reflection coating liquid of embodiment and anti-reflection coating
The formula of solvent-based system nano-coating liquid with anti-reflection function see the table below：
| Nano particle (wins wound Degussa Aerosil R812) | 1 part |
| Dispersant (wins wound Degussa Tego Dispers 655) | 1 part |
| Adhesion promoter (DOW CORNING Z-6030) | 0.2 part |
| Wetting agent (Bi Ke chemistry Byk-307) | 0.15 part |
| Pore-foaming agent (A Kema Chempol 317-8013) | 5 parts |
| Butyl acetate (chemical reagents corporation of Chinese Medicine group) | 94 parts |
Preparation method：
Dispersant and adhesion promoter are first dissolved in butyl acetate, nano particle is added under agitation, is mixed
After uniformly, is ground 12 hours in sand mill, obtain stable dispersion liquid.
Pore-foaming agent is dissolved in butyl acetate, then above-mentioned dispersion liquid and wetting agent is added in stirring condition successively, stirring is mixed
Solvent type nanometer anti-reflection coating liquid is obtained after closing uniformly.
By the nanometer anti-reflection coating liquid roller coating of gained in glass surface, by controlling roll coating speeds, by 500 DEG C, 2 minutes
Baking, it is respectively 150 nanometers~170 nanometers of anti-reflection coating to form film thickness in glass surface.The light transmission of gained anti-reflection film
Rate is higher than non-coated glass by 2.8%.
Embodiment 5 has the alcohol system nano-coating liquid II of anti-reflection function
Alcohol system nano-coating liquid II formulas with anti-reflection function see the table below：
Preparation method：
Dispersant and adhesion promoter are first dissolved in ethyl alcohol, nano particle is added under agitation, is uniformly mixed
Afterwards, it is ground 4 hours in sand mill, obtains stable dispersion liquid.
Pore-foaming agent is dissolved in ethyl alcohol, then above-mentioned dispersion liquid and wetting agent is added in stirring condition successively, is stirred
Alcohol system nanometer anti-reflection coating liquid is obtained after even.
By the nanometer anti-reflection coating liquid roller coating of gained in glass surface, by controlling roll coating speeds, by 600 DEG C, 2 minutes
Baking, it is respectively 150 nanometers~170 nanometers of anti-reflection coating to form film thickness in glass surface.The light transmission of gained anti-reflection film
Rate is higher than non-coated glass by 2.5%.
Comparative example 1 is free of the nanometer anti-reflection coating liquid and anti-reflection coating of adhesion promoter
The formula of nanometer anti-reflection coating liquid and anti-reflection coating without adhesion promoter see the table below：
Preparation method：
Dispersant is first dissolved in ethyl alcohol, nano particle is added under agitation, after mixing, is ground in sand mill
Mill 3 hours, obtains stable dispersion liquid.
Pore-foaming agent is dissolved in ethyl alcohol, then above-mentioned dispersion liquid and wetting agent is added in stirring condition successively, is stirred
Alcohol system nanometer anti-reflection coating liquid is obtained after even.
By the nanometer anti-reflection coating liquid roller coating of gained in glass surface, by controlling roll coating speeds, by 600 DEG C, 2 minutes
Baking, it is respectively 150 nanometers~170 nanometers of anti-reflection coating to form film thickness in glass surface.The light transmission of gained anti-reflection film
Rate is higher than non-coated glass by 2.5%.
The adhesive force of gained plated film can be tested by resistance to boiling brine (mass concentration 5%) and be characterized.Gained is coated with anti-reflection plating
The glass of film is immersed in brine, and brine is boiled, and keeps boil condition.The plated film of 1 gained of embodiment boiled by 1 hour
After saline sook, no discoloration and obscission show that the plated film of gained has high adhesive force, and comparative example to base material
The plated film of 1 gained is after 15 minutes boiling saline sooks, that is, the phenomenon that discoloration and partial exfoliation has occurred.This shows adhesive force
The introducing of accelerating agent can greatly improve the binding force of film and ground, to extend the service life of film.
Comparative example 2 is free of the nanometer anti-reflection coating liquid and anti-reflection coating of pore-foaming agent
The formula of nanometer anti-reflection coating liquid without pore-foaming agent see the table below：
| Nano particle (wins wound Degussa Aerosil 90) | 1 part |
| Dispersant (Bi Ke chemistry Disperbyk-161) | 0.5 part |
| Adhesion promoter (DOW CORNING, Z-6011) | 0.5 part |
| Wetting agent (Bi Ke chemistry Byk-3560) | 0.1 part |
| Absolute ethyl alcohol (chemical reagents corporation of Chinese Medicine group) | 94 parts |
Preparation method：
Dispersant and adhesion promoter are first dissolved in ethyl alcohol, nano particle is added under agitation, is uniformly mixed
Afterwards, it is ground 3 hours in sand mill, obtains stable dispersion liquid.
Pore-foaming agent is dissolved in ethyl alcohol, then above-mentioned dispersion liquid and wetting agent is added in stirring condition successively, is stirred
Alcohol system nanometer anti-reflection coating liquid is obtained after even.
By the nanometer anti-reflection coating liquid roller coating of gained in glass surface, by controlling roll coating speeds, by 600 DEG C, 2 minutes
Baking, it is respectively 150 nanometers~170 nanometers of anti-reflection coating to form film thickness in glass surface.The light transmission of gained anti-reflection film
Rate is only higher than non-coated glass by 1.6%.It is compared with embodiment 1 as can be seen that by being introduced into pore-foaming agent in film forming procedure
The antireflective effect of film can be greatly improved by forming spontaneous hole.
Claims (9)
1. a kind of nanometer anti-reflection coating liquid, composition of raw materials includes following components in parts by weight：Nano particle 0.1 ~ 5
80 ~ 99 parts of part, 0.1 ~ 20 part of pore-foaming agent, 0.1 ~ 5 part of adhesion promoter, 0.01 ~ 10 part of auxiliary agent and solvent；It is described
Pore-foaming agent include polyethylene oxide, polypropylene oxide, ethylene oxide/propylene oxide copolymer, polymethylacrylic acid（Ester）, it is poly-
Acrylic acid（Ester）, it is one or more in polyurethane and silicones；The auxiliary agent is dispersant and wetting agent.
2. nanometer anti-reflection coating liquid as described in claim 1, it is characterised in that：The solid content of the nanometer anti-reflection coating liquid
It is 1 ~ 30%；The initial size of the nano particle is 5 ~ 150 nanometers；The nano particle be nano silicon dioxide,
It is one or more in nano-titanium dioxide, nano magnesium fluoride, nano aluminium oxide.
3. nanometer anti-reflection coating liquid as described in claim 1, it is characterised in that：The adhesion promoter is silane coupled
It is one or more in agent, titanate coupling agent, zirconium ester coupling agent and aluminate coupling agent；The adhesion promoter
Dosage account for the 5 ~ 150% of the nanoparticle weight.
4. nanometer anti-reflection coating liquid as described in claim 1, it is characterised in that：The adhesion promoter is 3- aminopropans
Ethyl triethoxy silicane alkane, 3- TSL 8330s, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-shrink
Glycerine ether oxygen propyl triethoxysilane, γ-methacryloxypropyl trimethoxy silane and γ-methacryloxy
It is one or more in propyl-triethoxysilicane.
5. nanometer anti-reflection coating liquid as described in claim 1, it is characterised in that：The molecular structure of the dispersant wraps simultaneously
Contain：The macromolecular chain that there is the group of affinity and be easily completely solvated to inorganic pigment；Described having to inorganic pigment is affine
The group of power is one or more in carboxyl, carboxylate, phosphate-based, amino and ammonium root；The height being easily completely solvated
Strand is one or more in polyester, polyethers and polyacrylate；The dosage of the dispersant accounts for the nano particle
The 15 ~ 150% of total weight.
6. nanometer anti-reflection coating liquid as described in claim 1, it is characterised in that：The wetting agent can reduce coating liquid
Surface tension；The dosage of the wetting agent accounts for the 0 ~ 20% of the nanoparticle weight；The wetting agent is organosilicon
It is one or more in class compound, fluorocarbons and nonionic surfactant.
7. nanometer anti-reflection coating liquid as described in claim 1, it is characterised in that：The solvent be water, ethyl alcohol, isopropanol,
It is one or more in n-butanol, ethylene glycol, propylene glycol, acetone, 2- butanone, ethyl acetate, butyl acetate and dimethylbenzene.
8. a kind of preparation method of nanometer anti-reflection coating liquid as described in any one of claim 1 ~ 7 comprising Xia Shubu
Suddenly：
（1）Adhesion promoter and dispersant are dissolved in solvent, nano particle is added, ultrasound is carried out to it, then ball milling
Or sanded treatment, obtain dispersion liquid；
（2）Pore-foaming agent is dissolved in solvent, then under agitation, sequentially adds step（1）The dispersion liquid and wetting agent of gained,
After mixing, you can obtain nanometer anti-reflection coating liquid.
9. a kind of plated film with anti-reflection function, is made by following methods：Using the method for showering, dip-coating, spraying or roller coating
By the nanometer anti-reflection coating liquid even application described in any one of claim 1 ~ 8 after transparent substrate surface, baking
The plated film with anti-reflection function is made in transparent substrate surface；The baking condition is：300 ~ 900 DEG C of baking temperature dries
Roasting 1 ~ 10 minute time.
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| CN106634607A (en) * | 2016-11-08 | 2017-05-10 | 苏州蓝锐纳米科技有限公司 | Nano silica permeability-increasing liquid and preparation method thereof |
| CN107384199A (en) * | 2017-08-04 | 2017-11-24 | 伊婕 | A kind of vehicle glass coating liquid and preparation method thereof |
| CN108441927A (en) * | 2018-02-27 | 2018-08-24 | 德阳利源节能科技有限公司 | A kind of hot dip film liquid |
| CN108641423A (en) * | 2018-06-06 | 2018-10-12 | 彩虹集团新能源股份有限公司 | A kind of preparation method of photovoltaic glass coating liquid |
| CN112062477B (en) * | 2019-11-22 | 2022-09-16 | 焕澄(上海)新材料科技发展有限公司 | Perspective high-reflection coated glass and preparation method thereof |
| CN112795299A (en) * | 2020-12-30 | 2021-05-14 | 中建材（合肥）新能源有限公司 | Antireflection coating liquid, preparation method thereof and solar cell module |
| CN112919821A (en) * | 2021-02-09 | 2021-06-08 | 信义光伏产业(安徽)控股有限公司 | AR coating liquid, coated glass and preparation method thereof |
| CN113270041A (en) * | 2021-06-01 | 2021-08-17 | 北京航空航天大学 | Invisible display screen material, preparation method and application |
| CN114163137A (en) * | 2022-01-06 | 2022-03-11 | 山西日盛达太阳能科技股份有限公司 | Aqueous antireflection coating solution, preparation method thereof, photovoltaic glass and preparation method thereof |
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| CN102749666A (en) * | 2011-04-20 | 2012-10-24 | 国家纳米科学中心 | Preparation method for reflection-deducting coating |
| CN103951275A (en) * | 2014-04-08 | 2014-07-30 | 湖北桑夏太阳能产业有限公司 | Anti-reflection film and preparation method thereof |
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| CN102749666A (en) * | 2011-04-20 | 2012-10-24 | 国家纳米科学中心 | Preparation method for reflection-deducting coating |
| CN103951275A (en) * | 2014-04-08 | 2014-07-30 | 湖北桑夏太阳能产业有限公司 | Anti-reflection film and preparation method thereof |
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