KR101739076B1 - Antireflective coating composition and method for prepairing the same - Google Patents
Antireflective coating composition and method for prepairing the same Download PDFInfo
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- KR101739076B1 KR101739076B1 KR1020150157932A KR20150157932A KR101739076B1 KR 101739076 B1 KR101739076 B1 KR 101739076B1 KR 1020150157932 A KR1020150157932 A KR 1020150157932A KR 20150157932 A KR20150157932 A KR 20150157932A KR 101739076 B1 KR101739076 B1 KR 101739076B1
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- coating composition
- antireflective coating
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- 239000000203 mixture Substances 0.000 title claims abstract description 60
- 239000006117 anti-reflective coating Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000011230 binding agent Substances 0.000 claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000002834 transmittance Methods 0.000 claims abstract description 22
- 239000003960 organic solvent Substances 0.000 claims abstract description 21
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 8
- 125000003342 alkenyl group Chemical group 0.000 claims abstract description 4
- 125000003118 aryl group Chemical group 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 239000000758 substrate Substances 0.000 claims description 23
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 18
- 229960004592 isopropanol Drugs 0.000 claims description 14
- 238000006116 polymerization reaction Methods 0.000 claims description 14
- 230000006872 improvement Effects 0.000 claims description 13
- 239000011521 glass Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- OKIYQFLILPKULA-UHFFFAOYSA-N 1,1,1,2,2,3,3,4,4-nonafluoro-4-methoxybutane Chemical compound COC(F)(F)C(F)(F)C(F)(F)C(F)(F)F OKIYQFLILPKULA-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000012974 tin catalyst Substances 0.000 claims description 7
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 5
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 claims description 4
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 3
- 239000006059 cover glass Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 19
- 239000011248 coating agent Substances 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 11
- 239000010410 layer Substances 0.000 description 32
- -1 perfluoro compounds Chemical class 0.000 description 26
- 239000012975 dibutyltin dilaurate Substances 0.000 description 17
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 17
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 17
- 239000004205 dimethyl polysiloxane Substances 0.000 description 12
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 12
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 11
- 239000003054 catalyst Substances 0.000 description 10
- 230000003667 anti-reflective effect Effects 0.000 description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 8
- 239000012153 distilled water Substances 0.000 description 8
- 238000002454 metastable transfer emission spectrometry Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000003373 anti-fouling effect Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 6
- 239000011247 coating layer Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 229920000058 polyacrylate Polymers 0.000 description 5
- 239000003377 acid catalyst Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 229920001774 Perfluoroether Polymers 0.000 description 3
- 238000006482 condensation reaction Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- DFUYAWQUODQGFF-UHFFFAOYSA-N 1-ethoxy-1,1,2,2,3,3,4,4,4-nonafluorobutane Chemical compound CCOC(F)(F)C(F)(F)C(F)(F)C(F)(F)F DFUYAWQUODQGFF-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920002284 Cellulose triacetate Polymers 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 2
- CVBWTNHDKVVFMI-LBPRGKRZSA-N (2s)-1-[4-[2-[6-amino-8-[(6-bromo-1,3-benzodioxol-5-yl)sulfanyl]purin-9-yl]ethyl]piperidin-1-yl]-2-hydroxypropan-1-one Chemical compound C1CN(C(=O)[C@@H](O)C)CCC1CCN1C2=NC=NC(N)=C2N=C1SC(C(=C1)Br)=CC2=C1OCO2 CVBWTNHDKVVFMI-LBPRGKRZSA-N 0.000 description 1
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- MEWFSXFFGFDHGV-UHFFFAOYSA-N cyclohexyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C1CCCCC1 MEWFSXFFGFDHGV-UHFFFAOYSA-N 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- ZZNQQQWFKKTOSD-UHFFFAOYSA-N diethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)C1=CC=CC=C1 ZZNQQQWFKKTOSD-UHFFFAOYSA-N 0.000 description 1
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 description 1
- AHUXYBVKTIBBJW-UHFFFAOYSA-N dimethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C1=CC=CC=C1 AHUXYBVKTIBBJW-UHFFFAOYSA-N 0.000 description 1
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 239000012769 display material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 239000003361 porogen Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- ZUEKXCXHTXJYAR-UHFFFAOYSA-N tetrapropan-2-yl silicate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)OC(C)C ZUEKXCXHTXJYAR-UHFFFAOYSA-N 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- ALVYUZIFSCKIFP-UHFFFAOYSA-N triethoxy(2-methylpropyl)silane Chemical compound CCO[Si](CC(C)C)(OCC)OCC ALVYUZIFSCKIFP-UHFFFAOYSA-N 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- UMFJXASDGBJDEB-UHFFFAOYSA-N triethoxy(prop-2-enyl)silane Chemical compound CCO[Si](CC=C)(OCC)OCC UMFJXASDGBJDEB-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- LFRDHGNFBLIJIY-UHFFFAOYSA-N trimethoxy(prop-2-enyl)silane Chemical compound CO[Si](OC)(OC)CC=C LFRDHGNFBLIJIY-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/006—Anti-reflective coatings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The present invention relates to an antireflective coating comprising a binder polymerized by a sol-gel reaction from an alkoxysilane compound represented by the following general formula (1), an organic solvent and water, and having a pH of 4 to 5 Compositions and methods of making the same. The antireflective coating composition of the present invention has an excellent light transmittance and a low total reflectance, and thus has an excellent antireflection effect, an excellent durability, and a large area coating effect.
[Chemical Formula 1]
R 1 x Si (OR 2 ) 4 -x
Wherein R 1 is an alkyl group having 1 to 10 carbon atoms, an aryl group having 6 to 10 carbon atoms or an alkenyl group having 3 to 10 carbon atoms, R 2 is an alkyl group having 1 to 6 carbon atoms, x is 0? X <4 Lt; / RTI >
Description
The present invention relates to an antireflective coating composition and a method of manufacturing the same.
When the display is exposed to external light such as various lighting and natural light, the contrast is deteriorated due to the invisibility of the image formed in the display due to the reflected light to the eyes, which makes view of the screen difficult and the eyes feel fatigue Or headache. For this reason, the demand for reflection prevention is becoming very strong.
Also, antireflection coating technology is required in various fields other than the display field. For example, solar cells are performing anti-reflective coatings on the cover glass surface to improve conversion efficiency.
Thus, with emphasis on the need for anti-reflection, antireflection films have been developed in which a high refractive index layer and a low refractive layer are repeated in order to find a film structure having an anti-reflection effect in the visible light region, . Further, the anti-reflection film was developed in the form of a low refractive layer coated on the high refractive index layer, and it was found that the refractive index of the low refractive layer was superior to that of the high refractive index layer, There is still a difficulty in the design of the antireflection film that is included.
Korean Patent No. 913641 discloses a novel hybrid sol for the production of a wear resistant SiO 2 antireflective layer. In the sol-gel reaction, a porous structure is formed using a base catalyst. However, since the formed coating film has low strength, There is a problem that it is difficult to apply it on a desired glass substrate.
In Korean Patent No. 653585, an alkoxysilane containing a fluorine compound is used as an invention relating to "an antireflection film, a method of producing an antireflection film and an antireflection glass ", but fluoroalkoxysilane is sufficiently It is difficult to secure a low reflectance.
The object of the present invention is to provide a coating composition for antireflection which is excellent in light transmittance and low in total reflectance and thus excellent in antireflection effect.
Another object of the present invention is to provide an antireflective coating composition having excellent durability.
Another object of the present invention is to provide an antireflective coating composition excellent in antifouling property.
Another object to be solved by the present invention is to provide an antireflective coating composition which is easy to be coated on a large area.
The above and other objects of the present invention can be achieved by the present invention described below.
One aspect of the present invention relates to antireflective coating compositions.
Wherein the antireflective coating composition comprises a binder polymerized by an sol-gel reaction from an alkoxysilane compound represented by the following formula (1), an organic solvent and water,
which is prepared by neutralization so that the pH is 4 to 5;
[Chemical Formula 1]
R 1 x Si (OR 2 ) 4 -x
Wherein R 1 is an alkyl group having 1 to 10 carbon atoms, an aryl group having 6 to 10 carbon atoms or an alkenyl group having 3 to 10 carbon atoms, R 2 is an alkyl group having 1 to 6 carbon atoms, x is 0? X <4 Lt; / RTI >
The antireflective coating composition may include a pore-forming agent, which may be selected from the group consisting of perfluoro compounds, polydimethylsiloxane (PDMS), polyether-modified polydimethylsiloxane, Modified polyacrylates, and the like. [0035] The term " modified polyacrylate "
Wherein the perfluoro compound is a perfluoroether compound and the perfluoroether compound is selected from the group consisting of methoxy-nonafluorobutane (C 4 F 9 OCH 3 ) or ethoxy-nonafluorobutane ) (C 4 F 9 OC 2 H 5 ).
The pore-forming agent may be contained in an amount of 0.1 to 20 wt% of the binder.
The antireflective coating composition may include 100 parts by weight of the binder, 10 to 70 parts by weight of an organic solvent, and 0.05 to 0.5 parts by weight of dibutyltin diaurate (DBTDL).
The organic solvent may include at least one selected from the group consisting of methanol, ethanol, n-propyl alcohol, iso-propyl alcohol, and methyl cellosolve.
Another aspect of the invention is directed to a method of making an antireflective coating composition.
The antireflective coating composition may further include (S1) injecting 100 parts by weight of an organic solvent and 50-200 parts by weight of an alkoxysilane into the reactor and mixing the same. A step (S2) of raising the internal temperature of the reactor to 60 to 70; And a sol-gel reaction step (S3) of dropwise adding 50 to 150 parts by weight of water to a polymerization reaction for 5 to 7 hours to prepare a binder, wherein the sol- The pH change (? PH) before and after step S3 may be 0.5 or less.
In step (S1), a pore-forming agent may be further added together with the organic solvent and the alkoxysilane.
The method may further include a step (S4) of adding 50 to 500 parts by weight of an organic solvent and 0.05 to 0.5 parts by weight of a tin catalyst to 100 parts by weight of the binder.
Another aspect of the present invention relates to a substrate; And an antireflective layer formed on one surface of the substrate, wherein the antireflective layer is formed of the antireflective coating composition, the transmittance improvement degree of the antireflective layer is 2.0% or more in a wavelength range of 380 nm to 800 nm, A pencil hardness of 4H to 7H, and a contact angle of 80 to 110 [deg.].
The antireflection material may be a film for a display or a cover glass for a solar cell.
The antireflective coating composition of the present invention has a high transmittance improvement ratio and a low total reflectance, and thus has an excellent antireflection effect, an excellent durability and antifouling property, and an advantage of easy large-area coating.
FIG. 1 is a photograph of a reflection preventing layer made of the antireflective coating composition of Example 2, taken by a scanning electron microscope (SEM).
When the light travels through a certain medium and the refractive index reaches the interface with the other medium, a part or all of the light returns to the original medium. Reflection means that the amount of light transmitted as much as the amount of reflection And the output acting on the light source can be made unstable. Therefore, in the present invention, the coating layer for preventing such light reflection is defined as an anti-reflection layer.
In the present invention, the antireflective coating composition is defined as a composition for forming an antireflective layer on a substrate.
The antireflective coating composition according to one embodiment of the present invention includes an alkoxysilane compound represented by the following formula (1), an organic solvent, and a binder polymerized by sol-gel reaction from water.
[Chemical Formula 1]
R 1 x Si (OR 2 ) 4 -x
Wherein R 1 is an alkyl group having 1 to 10 carbon atoms, an aryl group having 6 to 10 carbon atoms or an alkenyl group having 3 to 10 carbon atoms, R 2 is an alkyl group having 1 to 6 carbon atoms, x is 0? X <4 Lt; / RTI >
The alkoxysilane compound represented by the general formula (1) may be at least one selected from the group consisting of tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetraisopropoxysilane, tetra-n-butoxysilane, tetra- -Butoxysilane, trimethoxysilane, triethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane , Isobutyltriethoxysilane, cyclohexyltrimethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, allyltrimethoxysilane allyltriethoxysilane, dimethyl Dimethoxy silane, dimethyl diethoxy silane, diphenyl dimethoxy silane, diphenyl diethoxy silane, and combinations thereof.
The antireflective coating composition of the present invention may contain 60 to 100% by weight of the binder prepared by a sol-gel reaction. In the sol-gel reaction, the alkoxysilane compound represented by the formula (1) is hydrolyzed and then subjected to dehydration condensation polymerization to form a siloxane compound.
In this case, in a conventional sol-gel reaction, an acid catalyst may be used to form a porous or linear network structure, or a basic catalyst may be used to form a branched clusters network structure. .
However, the present inventors have recognized that it is more advantageous to disperse the pores forming the porous structure in order to secure sufficient antireflection effect and light transmittance as well as excellent durability after curing of the antireflective coating composition. To this end, It was possible to prepare an antireflective coating composition without using an acid catalyst or a basic catalyst in a sol-gel reaction.
Accordingly, the antireflective coating composition of the present invention is prepared by a neutralization method, and the pH change (ΔPH) before and after the sol-gel reaction may be 0.5 or less, and the pH of the antireflective coating composition may be 4 to 5. In the present invention, the neutralization method is defined as a method of neutralizing the pH of the antireflective coating composition without using an acid catalyst or a basic catalyst in a sol-gel reaction.
The organic solvent used in the sol-gel reaction may be an aliphatic alcohol having 1 to 5 carbon atoms such as methanol, ethanol, n-propyl alcohol, iso-propyl alcohol, methyl cellosolve and the like. The organic solvent is essential for the hydrolysis and condensation reaction required for the sol-gel reaction and also suppresses the temperature rise in the initial exothermic reaction.
In addition, when the antireflective coating composition is coated on the substrate, the isophifyl alcohol may be further added to the post-reaction stage to improve the smoothness and control the content of the solid content. Specifically, the antireflective coating composition may include 50 to 500 parts by weight of isopropyl alcohol based on 100 parts by weight of the binder.
In another embodiment, the antireflective coating composition of the present invention may further comprise a tin catalyst as a curing catalyst. As the tin catalyst, dibutyltin diaurate (DBTDL) may be used.
The tin catalyst may be included in an amount of 0.05 to 0.5 parts by weight based on 100 parts by weight of the binder. In this range, the optical structure of the coating layer is not inhibited and the curing rate can be improved.
In another embodiment of the present invention, the antireflective coating composition may include a pore forming agent that further enhances the antireflective effect by better forming the porous structure of the nano-pores in the antireflective layer have. The pore-forming agent does not participate in the sol-gel reaction of the binder described above, and serves as a catalyst for promoting the formation of the porous structure.
The pore-forming agent may include at least one of a perfluoro compound, polydimethylsiloxane (PDMS), and modified polydimethylsiloxane.
As the perfluoro compound, a perfluoroether compound, specifically, methoxy-nonafluorobutane (C 4 F 9 OCH 3 ) or ethoxy-nonafluorobutane (C 4 F 9 OC 2 H 5 ) can be exemplified.
The modified polydimethylsiloxane may be a polyether-modified polydimethylsiloxane or a silicone-modified polyacrylates.
Examples of the polyether-modified polydimethylsiloxane include BYK-based compounds of BYK Corporation. The silicone-modified acrylate resin is represented by the following formula 2 and may be polydimethylsiloxane having a methacryl group at one end have.
(2)
The silicone modified acrylate resin has a number average molecular weight of 5,000 to 50,000 g / mol, preferably has a glass transition temperature of -100 to 120 ° C, and most preferably has a mono-meta It is a mono-methacrylic functional polysiloxane.
The pore-forming agent may be included in an amount of 0.1 to 20% by weight based on 100% by weight of the binder in the antireflective coating composition. If the amount is less than 0.1% by weight, the pore-forming effect is insignificant. If the amount is more than 20% by weight, the polymerization reaction is insufficient during the sol-gel reaction, so that the function as a binder for forming a coating layer is difficult.
Another aspect of the invention is directed to a method of making an antireflective coating composition. Since each component used in the production method to be described later is the same as that described above, the production method will be described in detail below.
According to an embodiment of the present invention, there is provided a process for preparing an antireflective coating composition, which comprises: (S1) charging 100 parts by weight of an organic solvent and 50-200 parts by weight of an alkoxysilane compound into a reactor; A step (S2) of raising the internal temperature of the reactor to 60 to 70 캜; And a sol-gel reaction step (S3) of dropwise adding 50 to 150 parts by weight of water to the reactor to conduct polymerization reaction for 5 to 7 hours to prepare a binder.
The temperature raising step (S2) may raise the temperature inside the reactor to 50 to 90 ° C, preferably 60 to 70 ° C. Under the above-mentioned temperature range, the polymerization reaction can proceed smoothly under the condition of the neutralization method. When the temperature is lower than 50 ° C, the polymerization reaction itself is difficult to start.
The sol-gel reaction in the step (S3) includes a hydrolysis reaction step of alkoxysilane, a water condensation reaction step, and an alcohol condensation reaction step.
In the present invention, the pH change (? PH) before and after the sol-gel reaction is 0.5 or less, and the pH of the prepared binder may be 4 to 5. The porous structure in the coating layer can be well formed under the above-mentioned pH conditions, so that an excellent antireflection effect can be exhibited.
According to another embodiment of the present invention, there is provided a method of preparing an antireflective coating composition, which comprises adding 50 to 500 parts by weight of an organic solvent and 0.05 to 0.5 parts by weight of a tin catalyst to 100 parts by weight of the binder, S4). When the organic solvent is further included, the coating property, the coating property, and the workability can be facilitated, and the curing rate can be improved when the tin catalyst is used.
The method for preparing an antireflective coating composition according to another embodiment of the present invention may further include a pore-forming agent together with an organic solvent and an alkoxysilane in step (S1). When the pore-forming agent is added to the step (S1), pores are formed at the same time as the polymerization reaction to form nanostructures of 100 nm or less which are easy to transmit light when the antireflection layer is formed.
According to another embodiment of the present invention, there is provided a method for preparing an antireflective coating composition, which comprises the steps of: dropping water in step (S3), adding a pore-forming agent after 3 hours of sol- 4 hours of additional polymerization reaction can be achieved.
The antireflective coating composition may be coated on a substrate and then cured to form an antireflective layer.
The substrate may be one selected from the group consisting of a polyethylene (PE) film, a polyethylene terephthalate (PET) film, a triacetylcellulose (TAC) film and a glass substrate, and preferably a glass substrate.
Examples of the coating method include spin coating, roll coating, bar coating, spray coating and dip coating. However, since the coating can be used in a large area with a uniform thickness, It is preferable to apply a coating.
The thickness of the coating layer formed on the substrate may be 90 to 100 nm. The light transmittance is high and the total reflection is reduced in the above-mentioned thickness range, and an excellent antireflection effect can be exhibited.
The antireflection layer made of the antireflective coating composition according to one embodiment of the present invention can have optical properties such as low reflectance, excellent transmittance improvement, no change in color difference upon transmission of light, Durability can be shown. In the present invention, the degree of improvement of the transmittance (%) means a value obtained by calculating the ratio of the initial transmittance (T 0 ) of the substrate to the transmittance (T 1 ) of the substrate having the antireflection layer formed thereon. (%) = (T 1 / T 0 ) X 100 .
Specifically, the transmittance improvement of the antireflection layer according to an embodiment of the present invention may be about 2.0% or more in a wavelength range of 380 nm to 800 nm, which is a visible light region.
The reflectance refers to the energy of the reflected light and the energy ratio of the incident light. The lower the reflectance of the antireflection film, the less the amount of the reflected light, and the less the influence of the light, the less the reflected light. The antireflection layer of the present invention maintains a transmittance improvement rate of about 2.0% or more before and after the coating, so that the antireflection function can be sufficiently exhibited.
In addition, the pencil hardness of the antireflection layer according to one embodiment of the present invention may be 4H to 7H. And can exhibit excellent durability in the above range.
The antireflective layer can be applied not only to the display material but also to an external solar cell module. Since the solar cell is exposed to the outside, it is required to have durability and antifouling property against external pollutants such as algae excrement, dust, and fine dust.
When the water is placed on a horizontal solid surface, it can be a droplet that maintains a constant lens shape. At this time, the surface of the water becomes a curved surface. The solid surface and the surface of the water can maintain a constant angle. Contact angle. In order to remove contaminants that are contaminated on the antireflection layer by natural rainfall, a contact angle to water is required to be about 80 DEG or more.
The contact angle of the antireflection layer with respect to water according to one embodiment of the present invention is excellent at an antifouling property of about 80 DEG or more, specifically about 80 DEG to about 110 DEG.
Hereinafter, the present invention will be described in more detail with reference to examples. However, these examples are presented for understanding of the present invention and should not be construed as limiting the scope of the present invention .
Example
In the example Specification of each component used
(A) Alkoxysilane compound
The alkoxysilane compounds include tetraethyl orthosilicate (TEOS) (Sigma Aldrich), triethoxymethylsilane (MTES) (Sigma Aldrich), tetramethyl orthosilicate (TMOS) (Sigma Aldrich ) And (3-Glycidyloxypropyl) trimethoxysilane (GPTMS) (Sigma Aldrich) were used.
(B) Organic solvent
Ethanol (Samseon Pure Chemical Co., Ltd.), and isopropyl alcohol (Samseon Pure Chemical Co., Ltd.) were used.
(C) Curing catalyst
Dibutyltin diaurate (DBTDL) (Sigma Aldrich) was used.
(D) Porogen
(d1) BYK 300 (BYK) was used as the polyether-modified polydimethylsiloxane.
(d2) Tego-5001 (Tego) was used as the silicone-modified polyacrylate.
(d3) was used as a purple butane ruoh a compound with methoxy nonafluoro (methoxy-nonafluorobutane) (C 4 F 9 OCH 3) (3M社HFE 7100).
How to measure property
? PH: The pH of the prepared antireflective coating composition was measured.
PH: The pH of the composition before and after the sol-gel reaction was measured, and the difference was calculated.
Transmittance improvement degree: The transmittance was measured according to the KS L2514 standard using a spectrophotometer (Shimadzu MPC-3100), and the degree of transmittance improvement was calculated from the initial transmittance (T 0 ) of the substrate and the transmittance (T 1 ), Respectively, and the ratio is calculated. Transmittance improvement rate (%) = (T 1 / T 0 ) X 100
Pencil hardness: The pencil hardness was measured with a pencil hardness tester (Shinto Scientific, Heidon) using a Mitsubishi evaluation pencil (UNI) at a load of 1 kg / cm 2 , 5 mm of 5 mm at a speed of 0.5 mm / sec, Respectively.
Contact angle: The contact angle was measured six times using distilled water with DAS-100 (Kruess) equipment and the average value was indicated.
Example One
To a 250 L Jacket Reactor was charged 60 g of ethanol, 15.5 g of tetraethylososilicate (TEOS), 5.5 g of triethoxymethylsilane (MTES), 32.0 g of tetramethylorthosilicate (TMOS) and (3-glycidyloxy Propyl) trimethoxysilane (GPTMS) were added and stirred, and the temperature inside the reactor was raised to 60 to 70 ° C. 55 g of distilled water was gradually added dropwise at a point of time when the internal temperature of the reactor reached 60 to 70 캜, followed by polymerization for 5 to 7 hours and cooling to room temperature (25 캜) to obtain a binder.
After mixing 0.05 g of dibutyltin dilaurate (DBTDL) with 20 g of the binder obtained above, 80 g of isopropyl alcohol was added to dilute the solution to prepare an antireflective coating composition.
The antireflective coating composition was coated on a glass substrate having a thickness of 3T by a roll coating method to form an antireflection layer having a thickness of 100 nm after curing.
Example 2
A 250 L jacket reactor was charged with 50 g of ethanol, 20.5 g of tetraethylorthosilicate (TEOS), 10.3 g of triethoxymethylsilane (MTES), 42.0 g of tetramethylorthosilicate (TMOS), 3 g of glycidyloxypropyl 5.7 g of trimethoxysilane (GPTMS) and 6.2 g of polyether-modified polydimethylsiloxane (d1) were charged and stirred, and the temperature inside the reactor was raised to 60 to 70 캜. At the time when the internal temperature of the reactor reached 60 to 70 캜, 61 g of distilled water was slowly added thereto by dropwise addition, and the mixture was polymerized for 5 to 7 hours and cooled to room temperature (25 캜) to obtain a binder.
After mixing 0.05 g of dibutyltin dilaurate (DBTDL) with 20 g of the binder obtained above, 80 g of isopropyl alcohol was added to dilute the solution to prepare an antireflective coating composition.
The antireflective coating composition was coated on a glass substrate having a thickness of 3T by a roll coating method to form an antireflection layer having a thickness of 100 nm after curing.
Example 3
A 250 L jacket reactor was charged with 50 g of ethanol, 14.3 g of tetraethylorthosilicate (TEOS), 6.2 g of triethoxymethylsilane (MTES), 15.0 g of tetramethylorthosilicate (TMOS), 3 g of glycidyloxypropyl ) 28.0 g of trimethoxysilane (GPTMS) and 7.4 g of silicone-modified polyacrylate (d2) were charged and stirred, and the internal temperature of the reactor was raised to 60 to 70 ° C. At the time when the internal temperature of the reactor reached 60 to 70 占 폚, distilled water (62 g) was slowly added thereto dropwise and the mixture was polymerized for 5 to 7 hours and cooled to room temperature (25 占 폚) to obtain a binder.
After mixing 0.05 g of dibutyltin dilaurate (DBTDL) with 20 g of the binder obtained above, 80 g of isopropyl alcohol was added to dilute the solution to prepare an antireflective coating composition.
The antireflective coating composition was coated on a glass substrate having a thickness of 3T by a roll coating method to form an antireflection layer having a thickness of 100 nm after curing.
Example 4
A 250 L jacket reactor was charged with 48 g of ethanol, 24 g of isopropyl alcohol, 31.0 g of tetraethylorthosilicate (TEOS), 6.9 g of triethoxymethylsilane (MTES), 14.2 g of tetramethylorthosilicate (TMOS) 13.8 g of glycidyloxypropyltrimethoxysilane (GPTMS) and 1.5 g of methoxy-nonafluorobutane (d3) were charged and stirred, and the internal temperature of the reactor was raised to 60 to 70 ° C. 55 g of distilled water was gradually added dropwise at a point of time when the internal temperature of the reactor reached 60 to 70 캜, followed by polymerization for 5 to 7 hours and cooling to room temperature (25 캜) to obtain a binder.
After mixing 0.05 g of dibutyltin dilaurate (DBTDL) with 20 g of the binder obtained above, 80 g of isopropyl alcohol was added to dilute the solution to prepare an antireflective coating composition.
The antireflective coating composition was coated on a glass substrate having a thickness of 3T by a roll coating method to form an antireflection layer having a thickness of 100 nm after curing.
Example 5
48 g of ethanol, 24 g of isopropyl alcohol, 31 g of tetraethylorthosilicate (TEOS), 6.9 g of triethoxymethylsilane (MTES), 14.2 g of tetramethylorthosilicate (TMOS) 13.8 g of glycidyloxypropyl) trimethoxysilane (GPTMS) was added and stirred, and the temperature inside the reactor was raised to 60 to 70 ° C. When the internal temperature of the reactor reached 60 to 70 ° C, distilled water (62 g) was slowly added thereto by dropwise addition. After 3 hours of polymerization, 1.5 g of methoxy-nonafluorobutane (d3) Respectively. Followed by polymerization for 3 to 4 hours, followed by cooling to room temperature (25 DEG C) to obtain a binder.
After mixing 0.05 g of dibutyltin dilaurate (DBTDL) with 20 g of the binder obtained above, 80 g of isopropyl alcohol was added to dilute the solution to prepare an antireflective coating composition.
The antireflective coating composition was coated on a glass substrate having a thickness of 3T by a roll coating method to form an antireflection layer having a thickness of 100 nm after curing.
Comparative Example One
To a 250 L jacket reactor was added 60 g of ethanol, 15.5 g of tetraethylorthosilicate (TEOS), 5.5 g of triethoxymethylsilane (MTES), 32.0 g of tetramethylorthosilicate (TMOS), 3 g of glycidyloxypropyl ) Trimethoxysilane (GPTMS) and 0.5 g of nitric acid (SAMCHUN 60%) as an acid catalyst were added and stirred, and the internal temperature of the reactor was raised to 60 to 70 ° C. 55 g of distilled water was gradually added dropwise at a point of time when the internal temperature of the reactor reached 60 to 70 캜, followed by polymerization for 5 to 7 hours and cooling to room temperature (25 캜) to obtain a binder.
After mixing 0.05 g of dibutyltin dilaurate (DBTDL) with 20 g of the binder obtained above, 80 g of isopropyl alcohol was added to dilute the solution to prepare an antireflective coating composition.
The antireflective coating composition was coated on a glass substrate having a thickness of 3T by a roll coating method to form an antireflection layer having a thickness of 100 nm after curing.
Comparative Example 2
To a 250 L jacket reactor was added 60 g of ethanol, 15.5 g of tetraethylorthosilicate (TEOS), 5.5 g of triethoxymethylsilane (MTES), 32.0 g of tetramethylorthosilicate (TMOS), 3 g of glycidyloxypropyl ) Trimethoxysilane (GPTMS) and 0.5 g of ammonium hydroxide (28% of purified gold) were charged into a basic catalyst, and the temperature inside the reactor was raised to 60 to 70 by stirring. At the time when the internal temperature of the reactor reached 60 to 70 占 폚, distilled water (55 g) was slowly added thereto dropwise and polymerization was carried out for 1 hour, followed by cooling to room temperature (25 占 폚) to obtain a binder.
After mixing 0.05 g of dibutyltin dilaurate (DBTDL) with 20 g of the binder obtained above, 80 g of isopropyl alcohol was added to dilute the solution to prepare an antireflective coating composition.
The antireflective coating composition was coated on a glass substrate having a thickness of 3T by a roll coating method to form an antireflection layer having a thickness of 100 nm after curing.
Improvement (%)
As seen from the results shown in Table 1, the antireflection layer prepared by the neutralization method and having a pH in the range of 4 to 5 has a high transmittance improvement degree and is excellent in antireflection effect and excellent in durability and antifouling property . On the other hand, in Comparative Example 1, as an example of using an acidic catalyst in the sol-gel reaction, the transmittance improvement degree is low and it is difficult to expect a sufficient antireflection effect. In Comparative Example 2, a basic catalyst was used in the sol-gel reaction, but it was found that durability was degraded and the contact angle of the water droplet was not measurable so that antifouling property was hardly secured.
Claims (13)
an antireflective coating composition characterized in that the antireflective coating composition is produced by a neutralization method so that the pH is 4 to 5;
[Chemical Formula 1]
R 1 x Si (OR 2 ) 4-x
Wherein R 1 is an alkyl group having 1 to 10 carbon atoms, an aryl group having 6 to 10 carbon atoms or an alkenyl group having 3 to 10 carbon atoms, R 2 is an alkyl group having 1 to 6 carbon atoms, x is 0? X <4 Lt; / RTI >
Wherein the methoxy-nonafluorobutane (C 4 F 9 OCH 3 ) is contained in an amount of 0.1 to 20 wt% of the binder.
100 parts by weight of the binder,
10 to 70 parts by weight of an organic solvent, and
0.05 to 0.5 parts by weight of dibutyltin diaurate (DBTDL).
Wherein the organic solvent comprises at least one selected from the group consisting of methanol, ethanol, n-propyl alcohol, iso-propyl alcohol, and methyl cellosolve.
A step (S2) of raising the internal temperature of the reactor to 60 to 70 캜;
And a sol-gel reaction step (S3) for dropwise adding 50 to 150 parts by weight of water to the polymerization reaction for 5 to 7 hours to prepare a binder,
The pH change (? PH) before and after the sol-gel reaction step (S3) is 0.5 or less,
Wherein methoxy-nonafluorobutane (C 4 F 9 OCH 3 ) is further added as a pore-forming agent together with the organic solvent and the alkoxysilane in the step (S1) / RTI > to < RTI ID = 0.0 >
Further comprising the step (S4) of adding 50 to 500 parts by weight of an organic solvent and 0.05 to 0.5 parts by weight of a tin catalyst to 100 parts by weight of the binder thus prepared, followed by mixing (S4) Way.
And an antireflection layer formed on one side of the substrate,
Wherein the antireflection layer is made of the antireflective coating composition of any one of claims 1, 4, and 5,
The transmittance improvement degree of the antireflection layer is 2.0% or more in the wavelength range of 380 nm to 800 nm,
A pencil hardness of 4H to 7H,
Wherein the contact angle is in the range of 80 DEG to 110 DEG.
The substrate is a glass substrate,
A solar cell cover glass.
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