JP6879929B2 - 光機能性膜およびその製造方法 - Google Patents
光機能性膜およびその製造方法 Download PDFInfo
- Publication number
- JP6879929B2 JP6879929B2 JP2017551125A JP2017551125A JP6879929B2 JP 6879929 B2 JP6879929 B2 JP 6879929B2 JP 2017551125 A JP2017551125 A JP 2017551125A JP 2017551125 A JP2017551125 A JP 2017551125A JP 6879929 B2 JP6879929 B2 JP 6879929B2
- Authority
- JP
- Japan
- Prior art keywords
- layer
- refractive index
- polysiloxane
- film
- group
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- -1 polysiloxane Polymers 0.000 claims description 145
- 229920001296 polysiloxane Polymers 0.000 claims description 101
- 239000000203 mixture Substances 0.000 claims description 68
- 229920000642 polymer Polymers 0.000 claims description 46
- 239000000463 material Substances 0.000 claims description 43
- 239000002105 nanoparticle Substances 0.000 claims description 40
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 35
- 239000002904 solvent Substances 0.000 claims description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 27
- 239000003960 organic solvent Substances 0.000 claims description 23
- 125000005372 silanol group Chemical group 0.000 claims description 23
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 23
- 229910044991 metal oxide Inorganic materials 0.000 claims description 22
- 150000004706 metal oxides Chemical class 0.000 claims description 22
- 229910000077 silane Inorganic materials 0.000 claims description 21
- 239000003054 catalyst Substances 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 17
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 13
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 11
- 125000003545 alkoxy group Chemical group 0.000 claims description 10
- 239000004065 semiconductor Substances 0.000 claims description 10
- 239000003125 aqueous solvent Substances 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 230000016507 interphase Effects 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 125000003118 aryl group Chemical group 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 125000003342 alkenyl group Chemical group 0.000 claims description 2
- 125000006165 cyclic alkyl group Chemical group 0.000 claims description 2
- 125000001153 fluoro group Chemical group F* 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims 1
- 239000010408 film Substances 0.000 description 140
- 239000010410 layer Substances 0.000 description 132
- 238000000576 coating method Methods 0.000 description 45
- 239000011248 coating agent Substances 0.000 description 41
- 238000006243 chemical reaction Methods 0.000 description 32
- 239000011521 glass Substances 0.000 description 32
- 238000002834 transmittance Methods 0.000 description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 19
- 230000003287 optical effect Effects 0.000 description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 238000011282 treatment Methods 0.000 description 15
- 239000002585 base Substances 0.000 description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- 239000007810 chemical reaction solvent Substances 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 10
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000008859 change Effects 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001723 curing Methods 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 230000002209 hydrophobic effect Effects 0.000 description 6
- 125000004430 oxygen atom Chemical group O* 0.000 description 6
- 239000003444 phase transfer catalyst Substances 0.000 description 6
- 125000001424 substituent group Chemical group 0.000 description 6
- 239000004094 surface-active agent Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 5
- 150000003863 ammonium salts Chemical class 0.000 description 5
- 238000013329 compounding Methods 0.000 description 5
- 238000006482 condensation reaction Methods 0.000 description 5
- 238000000605 extraction Methods 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 239000002609 medium Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000000693 micelle Substances 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 238000006386 neutralization reaction Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 4
- 239000012074 organic phase Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 3
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 3
- 239000003729 cation exchange resin Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000013007 heat curing Methods 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 230000001771 impaired effect Effects 0.000 description 3
- 238000010030 laminating Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 230000003472 neutralizing effect Effects 0.000 description 3
- 239000012044 organic layer Substances 0.000 description 3
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 3
- 150000004023 quaternary phosphonium compounds Chemical class 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 3
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- XLLIQLLCWZCATF-UHFFFAOYSA-N 2-methoxyethyl acetate Chemical compound COCCOC(C)=O XLLIQLLCWZCATF-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 229910002808 Si–O–Si Inorganic materials 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000005456 alcohol based solvent Substances 0.000 description 2
- 125000005370 alkoxysilyl group Chemical group 0.000 description 2
- 150000005215 alkyl ethers Chemical class 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 239000002280 amphoteric surfactant Substances 0.000 description 2
- 150000008064 anhydrides Chemical class 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N anhydrous diethylene glycol Natural products OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 150000007514 bases Chemical class 0.000 description 2
- 229960003237 betaine Drugs 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 150000003983 crown ethers Chemical class 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 239000003759 ester based solvent Substances 0.000 description 2
- 239000004210 ether based solvent Substances 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 150000007529 inorganic bases Chemical class 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 239000005453 ketone based solvent Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- CLZGJKHEVKJLLS-UHFFFAOYSA-N n,n-diheptylheptan-1-amine Chemical compound CCCCCCCN(CCCCCCC)CCCCCCC CLZGJKHEVKJLLS-UHFFFAOYSA-N 0.000 description 2
- DIAIBWNEUYXDNL-UHFFFAOYSA-N n,n-dihexylhexan-1-amine Chemical compound CCCCCCN(CCCCCC)CCCCCC DIAIBWNEUYXDNL-UHFFFAOYSA-N 0.000 description 2
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 description 2
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- YKYONYBAUNKHLG-UHFFFAOYSA-N propyl acetate Chemical compound CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 150000004756 silanes Chemical class 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 2
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 2
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 2
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- FFJCNSLCJOQHKM-CLFAGFIQSA-N (z)-1-[(z)-octadec-9-enoxy]octadec-9-ene Chemical compound CCCCCCCC\C=C/CCCCCCCCOCCCCCCCC\C=C/CCCCCCCC FFJCNSLCJOQHKM-CLFAGFIQSA-N 0.000 description 1
- BOGFHOWTVGAYFK-UHFFFAOYSA-N 1-[2-(2-propoxyethoxy)ethoxy]propane Chemical compound CCCOCCOCCOCCC BOGFHOWTVGAYFK-UHFFFAOYSA-N 0.000 description 1
- RRQYJINTUHWNHW-UHFFFAOYSA-N 1-ethoxy-2-(2-ethoxyethoxy)ethane Chemical compound CCOCCOCCOCC RRQYJINTUHWNHW-UHFFFAOYSA-N 0.000 description 1
- LIPRQQHINVWJCH-UHFFFAOYSA-N 1-ethoxypropan-2-yl acetate Chemical compound CCOCC(C)OC(C)=O LIPRQQHINVWJCH-UHFFFAOYSA-N 0.000 description 1
- DMFAHCVITRDZQB-UHFFFAOYSA-N 1-propoxypropan-2-yl acetate Chemical compound CCCOCC(C)OC(C)=O DMFAHCVITRDZQB-UHFFFAOYSA-N 0.000 description 1
- IHJUECRFYCQBMW-UHFFFAOYSA-N 2,5-dimethylhex-3-yne-2,5-diol Chemical compound CC(C)(O)C#CC(C)(C)O IHJUECRFYCQBMW-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- SVONRAPFKPVNKG-UHFFFAOYSA-N 2-ethoxyethyl acetate Chemical compound CCOCCOC(C)=O SVONRAPFKPVNKG-UHFFFAOYSA-N 0.000 description 1
- CRWNQZTZTZWPOF-UHFFFAOYSA-N 2-methyl-4-phenylpyridine Chemical compound C1=NC(C)=CC(C=2C=CC=CC=2)=C1 CRWNQZTZTZWPOF-UHFFFAOYSA-N 0.000 description 1
- CEBKHWWANWSNTI-UHFFFAOYSA-N 2-methylbut-3-yn-2-ol Chemical compound CC(C)(O)C#C CEBKHWWANWSNTI-UHFFFAOYSA-N 0.000 description 1
- YEYKMVJDLWJFOA-UHFFFAOYSA-N 2-propoxyethanol Chemical compound CCCOCCO YEYKMVJDLWJFOA-UHFFFAOYSA-N 0.000 description 1
- NUYADIDKTLPDGG-UHFFFAOYSA-N 3,6-dimethyloct-4-yne-3,6-diol Chemical compound CCC(C)(O)C#CC(C)(O)CC NUYADIDKTLPDGG-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- RAXXELZNTBOGNW-UHFFFAOYSA-O Imidazolium Chemical compound C1=C[NH+]=CN1 RAXXELZNTBOGNW-UHFFFAOYSA-O 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical class C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000003849 aromatic solvent Substances 0.000 description 1
- FWLORMQUOWCQPO-UHFFFAOYSA-N benzyl-dimethyl-octadecylazanium Chemical class CCCCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 FWLORMQUOWCQPO-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- XGZGKDQVCBHSGI-UHFFFAOYSA-N butyl(triethoxy)silane Chemical compound CCCC[Si](OCC)(OCC)OCC XGZGKDQVCBHSGI-UHFFFAOYSA-N 0.000 description 1
- SXPLZNMUBFBFIA-UHFFFAOYSA-N butyl(trimethoxy)silane Chemical compound CCCC[Si](OC)(OC)OC SXPLZNMUBFBFIA-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- KQAHMVLQCSALSX-UHFFFAOYSA-N decyl(trimethoxy)silane Chemical compound CCCCCCCCCC[Si](OC)(OC)OC KQAHMVLQCSALSX-UHFFFAOYSA-N 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 229940019778 diethylene glycol diethyl ether Drugs 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-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
- MYEJNNDSIXAGNK-UHFFFAOYSA-N ethyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](CC)(OC(C)C)OC(C)C MYEJNNDSIXAGNK-UHFFFAOYSA-N 0.000 description 1
- 229910001940 europium oxide Inorganic materials 0.000 description 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 description 1
- CZWLNMOIEMTDJY-UHFFFAOYSA-N hexyl(trimethoxy)silane Chemical compound CCCCCC[Si](OC)(OC)OC CZWLNMOIEMTDJY-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229960002050 hydrofluoric acid Drugs 0.000 description 1
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 125000003010 ionic group Chemical group 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- HLXDKGBELJJMHR-UHFFFAOYSA-N methyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](C)(OC(C)C)OC(C)C HLXDKGBELJJMHR-UHFFFAOYSA-N 0.000 description 1
- QXLPXWSKPNOQLE-UHFFFAOYSA-N methylpentynol Chemical compound CCC(C)(O)C#C QXLPXWSKPNOQLE-UHFFFAOYSA-N 0.000 description 1
- ZUZLIXGTXQBUDC-UHFFFAOYSA-N methyltrioctylammonium Chemical class CCCCCCCC[N+](C)(CCCCCCCC)CCCCCCCC ZUZLIXGTXQBUDC-UHFFFAOYSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000006353 oxyethylene group Chemical group 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 1
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical class CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-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
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
- GIHPVQDFBJMUAO-UHFFFAOYSA-N tributoxy(ethyl)silane Chemical compound CCCCO[Si](CC)(OCCCC)OCCCC GIHPVQDFBJMUAO-UHFFFAOYSA-N 0.000 description 1
- GYZQBXUDWTVJDF-UHFFFAOYSA-N tributoxy(methyl)silane Chemical compound CCCCO[Si](C)(OCCCC)OCCCC GYZQBXUDWTVJDF-UHFFFAOYSA-N 0.000 description 1
- WUMSTCDLAYQDNO-UHFFFAOYSA-N triethoxy(hexyl)silane Chemical compound CCCCCC[Si](OCC)(OCC)OCC WUMSTCDLAYQDNO-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
- BOVWGKNFLVZRDU-UHFFFAOYSA-N triethoxy(trifluoromethyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)F BOVWGKNFLVZRDU-UHFFFAOYSA-N 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- JLGNHOJUQFHYEZ-UHFFFAOYSA-N trimethoxy(3,3,3-trifluoropropyl)silane Chemical compound CO[Si](OC)(OC)CCC(F)(F)F JLGNHOJUQFHYEZ-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
- ORVBHOQTQDOUIW-UHFFFAOYSA-N trimethoxy(trifluoromethyl)silane Chemical compound CO[Si](OC)(OC)C(F)(F)F ORVBHOQTQDOUIW-UHFFFAOYSA-N 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/111—Anti-reflection coatings using layers comprising organic materials
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
- C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3405—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of organic materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/398—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing boron or metal atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/28—Treatment by wave energy or particle radiation
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
-
- 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
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/85—Arrangements for extracting light from the devices
- H10K50/858—Arrangements for extracting light from the devices comprising refractive means, e.g. lenses
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
- C03C2217/475—Inorganic materials
- C03C2217/478—Silica
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/73—Anti-reflective coatings with specific characteristics
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/73—Anti-reflective coatings with specific characteristics
- C03C2217/732—Anti-reflective coatings with specific characteristics made of a single layer
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/73—Anti-reflective coatings with specific characteristics
- C03C2217/734—Anti-reflective coatings with specific characteristics comprising an alternation of high and low refractive indexes
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/90—Other aspects of coatings
- C03C2217/91—Coatings containing at least one layer having a composition gradient through its thickness
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/70—Siloxanes defined by use of the MDTQ nomenclature
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
-
- 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
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
- H01L31/02168—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells the coatings being antireflective or having enhancing optical properties for the solar cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/44—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the coatings, e.g. passivation layer or anti-reflective coating
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/85—Arrangements for extracting light from the devices
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Optics & Photonics (AREA)
- Geochemistry & Mineralogy (AREA)
- Composite Materials (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Wood Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Laminated Bodies (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Silicon Polymers (AREA)
Description
これら、ガラス表面への映り込み、光取り込み効率または光取り出し効率の低下は、屈折率が異なる2つの層の界面で起こる反射に起因している。このような反射は、これらの問題の他にも、層内での多重反射による透過率の波長依存性を引き起こすこともある。
Rf=(n1−n0)2/(n1+n0)2
この反射防止膜により、低屈折率層(たとえば空気層)と反射防止膜との界面における反射と、反射防止膜と高屈折率層(たとえばガラス)との界面における反射との光学干渉により反射率を低減させることができる。上記条件で、反射防止膜に最適な屈折率n2は
n2=(n1/n0)1/2
であらわされる。たとえば、空気層とガラスとの間には、屈折率1.22の非常に低い屈折率層が要求される。さらに、低屈折率層と高屈折率層の各々の反射光を逆位相にするためには、低屈折率層の膜厚はλ/4(ここでλは入射光波長である)であり、波長を可視光域の中心のλ=550nmに設定した場合の最適膜厚は0.14μmである。
しかし、膜厚を完全に一定にし、反射光を完全に逆位相にして打ち消し合わせるのは困難であり、また、単一の波長の光ではなく、複数の波長の光等を用いることも想定され、反射防止膜を用いた場合に透過率の波長依存性を小さくすることは課題である。
また、本発明による光機能性膜は、生産性にすぐれ、大面積の膜を形成可能であり、経済性および汎用性の面においても優れたものである。
本発明による光機能性膜は、シリカ質材料を含んでなる。ここでシリカ質材料とは、シロキサンを主体とした材料であり、このようなシリカ質材料を含む光機能性膜の形成方法は後述する。
したがって、この光機能性膜の表面Aおよび表面Bは、種々の媒体と接触するように配置される。たとえば、太陽電池などの受光素子の表面に用いられる場合には、通常、屈折率の高い表面Aが半導体素子の表面に接触し、屈折率の低い表面Bは空気に接触する。また、本発明による光機能性膜が発光素子の表面に用いられる場合には、発光素子の発光面に屈折率の高い表面Aが発光素子の表面に接触し、屈折率の低い表面Bは、さらに光機能性膜の上に設けられたガラス保護膜に接触することがある。
このとき、表面Aに接触する媒体Xの屈折率がnXであり、表面Bに接触する媒体Yの屈折率がnYであるとき、
nY≦nB<nA≦nX
の関係を満たすことが好ましい。特に、表面Bが空気に接触している時には、
1≦nB<nA≦nX
であることが好ましい。そして、一表面の屈折率と、その表面に接触する媒体の屈折率との差が大きいと、その接触界面において光反射が大きくなる。したがって、nYとnBの差、およびnAとnXの差は小さいことが好ましい。理想的には、nB−nY=0、nx−nA=0である。なお、nAとnXの差が1%未満であれば、nA<nXであったとしても、本発明の効果は実質的に失われない。ここで、各屈折率は、光を利用する場合は、波長が555nmの光に対するものである。
本発明による光機能性膜は、任意の方法により形成させることができる。形成方法に応じて、たとえば図2〜図4に示されるような屈折率の変化を示す光機能性膜を形成させることができるが、特に図2に示されるような屈折率変化を示す光機能性膜を形成させることが比較的簡便であり、生産性に優れている。
R11 n1Si(OR12)4−n1 (1)(式中、
R11は、任意のメチレンが酸素で置き換えられてもよい炭素数1〜20の直鎖状、分岐状あるいは環状のアルキル基、または炭素数6〜20で任意の水素がフッ素で置き換えられていてもよいアリール基を表し、
R12は、水素または炭素数1〜10のアルキル基、好ましくは炭素数1〜6のアルキル基、を表し、
n1は0〜2を表す。)
であらわされるシラン化合物を、酸性あるいは塩基性触媒の存在下で加水分解・縮合させて得られるものである。このようなポリシロキサンからは、一般に屈折率が1.30〜1.60程度のシリカ質材料を得ることができる。
これらの中で、メチルトリメトキシシラン、メチルトリエトキシシラン、フェニルトリメトキシシラン、フェニルトリエトキシシランは、入手しやすく好ましい化合物である。
このような複合体を含む被膜を焼成すると、ナノ粒子の周囲に空隙が形成されるのである。このような複合体を用いることにより、空隙率に応じて屈折率が1.05〜1.40程度のシリカ質材料を得ることができる。
そのほか、ユーロピウム酸化物を用いた場合には、硬化膜に蛍光特性を付与することができ、酸化亜鉛を用いた場合は、UV吸収特性が付与され、酸化ホウ素を用いた場合は、フィルムの誘電率が低くなり、酸化アルミニウムを用いた場合は、赤外吸収特性が付与される。これらの特性改善または特性付与の観点から、チタン、ジルコニウム、亜鉛、ホウ素、またはアルミニウムの酸化物を用いることが好ましい。
MxOy(OR3)z (3)(式中、
MはTi、Zr、Eu、Zn、B、Al、Ta、およびHfからなる群から選択される元素であり、
R3は、水素、またはC1〜C10の、好ましくはC1〜C6の、アルキル基またはアルケニル基であり、
2y+z=x×[Mの価数]を満たす)
本発明による光機能性膜は光反射が少ないため、半導体素子などの表面に用いるのに有用である。そして、シリカ質材料から形成されていることから、透過率、強度、誘電率などにも優れている。このため、本発明による光機能性膜を具備した半導体素子、たとえば太陽電池、LED及びOLEDなどは優れた特性を示すものである。そして、特に発光素子や太陽電池などの光を利用する素子には、高温耐性、環境耐性、光耐性、または化学薬品耐性等が要求されるため、シリカ質材料から形成されている本発明による光機能性膜は特に有用である。
撹拌機、温度計、冷却管を備えた2Lのフラスコ中で、水酸化ナトリウム20g、イソプロピルアルコール(以下、IPAという)300ml、および水13.5gを混合して反応溶媒を調製し、10℃に維持した。さらに、メチルトリメトキシシラン68gを加え混合溶液を調製した。その混合溶液を10℃にて滴下ロートを用いて反応溶媒に滴下し、10℃に維持しながら2時間撹拌した後、10%HCl水溶液を加え中和した。反応液にトルエン200ml、および水300mlを添加して振とうした後、2層に分離させた。
得られた有機層を減圧下濃縮することで溶媒を除去し、濃縮物に固形分濃度10重量%なるようにPGMEAを添加して、メチルシルセスキオキサン含有組成物A(以下、組成物Aという)を調整した。得られたメチルシルセスキオキサンの平均重量分子量(ポリスチレン換算)は3,562であった。
撹拌機、温度計、冷却管を備えた2Lのフラスコ中で、25重量%テトラメチルアンモニウムヒドロキシド水溶液36.5g、IPA300ml、および水1.5gを混合して反応溶媒を調製し、10℃に維持した。さらに、フェニルトリメトキシシラン44.6g、メチルトリメトキシシラン34.1g、およびテトラメトキシシラン3.8gの混合溶液を調製した。その混合溶液を10℃にて滴下ロートを用いて反応溶媒に滴下し、10℃に維持しながら2時間撹拌した後、10%HCl水溶液を加え中和した。反応液にトルエン200ml、および水300mlを添加して振とうした後、2層に分離させた。得られた有機層を減圧下濃縮することで溶媒を除去し、濃縮物に固形分濃度10重量%なるようにPGMEAを添加して、メチルフェニルシルセスキオキサン含有組成物B(以下、組成物Bという)を含む溶液を調整した。得られたメチルフェニルシルセスキオキサンの平均重量分子量(ポリスチレン換算)は2,180であった。
ガラス基板の表面に、組成物Aを塗布し、100℃90秒間プリベーク後、300℃1時間加熱して、厚さ1μmの被膜を形成させた。ガラス基板の屈折率は1.48、被膜の屈折率は1.38であった。
このとき、透過率は図6に示す通りであり、450nmから800nmの平均は、93.3%であった。これは、透過光が、入射光とガラスの界面の反射(屈折率より計算した理論値3.87%)、ガラスの界面と被膜の界面の反射(理論値0.15%)、および被膜と空気の界面の反射(理論値2.55%)によって減少した結果と考えられる。なお、透過率の理論値は92.38%である。
ガラス基板の表面に、組成物Bを塗布し、100℃90秒間プリベーク後、300℃30分間加熱して、厚さ1μmの被膜を形成させた。被膜の屈折率は1.49であった。
このとき、透過率は図6に示す通りであり、450nmから800nmの透過率の平均は92.3%であった。これは、透過光が、入射光とガラスの界面の反射(屈折率より計算した理論値3.87%)、ガラスの界面と被膜の界面の反射(理論値0.00%)、および被膜と空気の界面の反射(理論値3.75%)によって減少した結果と考えられる。
なお、透過率の理論値は92.23%である。
また、図6に示すように、比較例2では、ガラス単独のときと同様に、波長依存はほとんど確認されなかった。これは、被膜の屈折率はガラスの屈折率とほぼ同等のため、ガラスと被膜の間で反射が起こらず、反射光の干渉が起こらなかったためと推測される。
ガラス基板の表面に、組成物Bを500nmの厚さとなるように塗布し、150℃90秒間加熱して第1層を形成させた。次いで、組成物Aを500nmの厚さとなるように塗布し、200℃90秒間プリベーク後、300℃1時間加熱して、第1層および第2層を完全に硬化させた。すなわち、異なる屈折率を有する第1層と第2層とが積層され、それらの界面部分が相溶した光機能性膜を形成させた。
このとき、透過率は図7に示す通りであり、450nmから800nmの透過率の平均は93.2%であった。これは、透過光が、入射光とガラスの界面の反射(屈折率より計算した理論値3.87%)、ガラスの界面と光機能性膜の界面の反射(光機能性膜のガラスに近い部分の屈折率を1.49とすると、理論値0.00%)、および光機能性膜と空気の界面の反射(光機能性膜の空気に近い部分の屈折率を1.38とすると、理論値2.55%)によって減少した結果と考えられる。なお、透過率の理論値は93.58%である。
また、図7に示すように、透過率の波長依存はほとんど観測されなかった。これは、これは、被膜の屈折率はガラスの屈折率とほぼ同等のため、ガラスと被膜の間で反射が起こらず、反射光の干渉が起こらなかったためと推測される。
以上より、実施例1は、透過率に優れ、かつ透過率が波長依存性のない優れた光機能性膜であると言える。
第一層の組成物B塗布直後の加熱温度以外は実施例1と同様にして、光機能性膜を形成した。参考例1、2、および3の加熱温度は、それぞれ130℃、170℃、および200℃であった。
このとき、透過率は図8に示す通りであり、450nmから800nmの透過率の平均は実施例と同等であった。
参考例1は、図8に示すように透過率の波長依存性が若干見られた。これは、組成物B塗布直後の加熱温度が低いために、第2層の組成物Aの塗布時に、第1層の一部が溶解してしまい、結果として、実施例1で認められる程度の構造による波長依存性改良効果が得られなかったためと考えられる。
透過率の波長依存性は少ない光機能性膜が求められるので、第一層塗布後の加熱温度の最適化が必要と考えられる。
Claims (8)
- シリカ質材料を含んでなる光機能性膜の製造方法であって、
前記シリカ質材料が、シラノール基を有するポリシロキサンを原料として形成されたものであり、
前記光機能性膜は、基材の上にポリシロキサンと溶媒とを含む組成物を塗布し、100〜200℃で加熱することにより表面の難溶化処理をして第1層を形成させる第1層形成工程、前記第1層の表面に前記ポリシロキサンとは異なるポリシロキサンと、前記溶媒と同一または異なる溶媒とを含む組成物を塗布して第2層を形成させる第2層形成工程、および前記第1層および前記第2層を加熱して硬化させる加熱工程を含んでなり、前記第2層形成工程開始後から加熱工程終了までの間に、150℃以上で加熱することにより前記第1層と前記第2層の接触部分を相溶化させることを含んでなることによって製造され、
前記光機能性膜の一方の表面Aの光に対する屈折率nAが、反対側表面Bの光に対する屈折率nBに対して大きく、前記表面Aから前記表面Bまで、光に対する屈折率が連続的に減少するものであり、
前記表面Aに接触する媒体Xの屈折率がnXであり、前記表面Bに接触する媒体Yの屈折率がnYであるとき、
nY≦nB<nA≦nXの関係を満たすことを特徴とする光機能性膜の製造方法。 - 前記ポリシロキサンが、一般式(1)
R11 nSi(OR12)4−n (1)
(式中、
R11は、任意のメチレンが酸素で置き換えられてもよい炭素数1〜20の直鎖状、分岐状あるいは環状のアルキル基、または炭素数6〜20で任意の水素がフッ素で置き換えられていてもよいアリール基を表し、
R12は、炭素数1〜6のアルキル基を表し、
nは0または1または2を表す。)
であらわされるシラン化合物を、酸性あるいは塩基性触媒の存在下で加水分解・縮合させて得られるものである、請求項1に記載の方法。 - 前記ポリシロキサンが、シラノール基を有するシロキサンポリマー、シラノール基を有するシランモノマー、またはそれらの混合物と、表面に水酸基またはアルコキシ基を有するケイ素酸化物ナノ粒子とを、水性溶媒と有機性溶媒との混合溶媒中、相間移動触媒の存在下で反応させることにより得られることを特徴とするケイ素酸化物ナノ粒子とシロキサンポリマーの複合体である、請求項1または2に記載の方法。
- 前記ポリシロキサンが、シラノール基を有するシロキサンポリマー、シラノール基を有するシランモノマー、またはそれらの混合物と、表面に水酸基またはアルコキシ基を有する金属酸化物ナノ粒子とを、水性溶媒と有機性溶媒との混合溶媒中、相間移動触媒の存在下で反応させることにより得られることを特徴とする金属酸化物ナノ粒子とシロキサンポリマーとの複合体である、請求項1〜3のいずれか一項に記載の方法。
- 前記金属酸化物ナノ粒子が、下記一般式(3)
MxOy(OR3)z (3)
(式中、
MはTi、Zr、Eu、Zn、B、Al、Ta、およびHfからなる群から選択される元素であり、
R3は、水素、またはC1〜C10のアルキル基またはアルケニル基であり、
2y+z=x×[Mの価数]を満たす)
で表される、請求項4に記載の方法。 - 基材表面に、請求項1〜5のいずれか1項に記載の方法で製造された光機能性膜を具備してなる、半導体素子の製造方法。
- 前記光機能性膜の表面Aが前記基板表面に接触している、請求項6に記載の方法。
- 前記基板の屈折率nSが、表面Aの屈折率nAよりも大きい、請求項7に記載の方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2015094323A JP2016212193A (ja) | 2015-05-01 | 2015-05-01 | 光機能性膜およびその製造方法 |
JP2015094323 | 2015-05-01 | ||
PCT/EP2016/000608 WO2016177448A1 (en) | 2015-05-01 | 2016-04-13 | Optical functional film and method for producing the same |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2018517162A JP2018517162A (ja) | 2018-06-28 |
JP6879929B2 true JP6879929B2 (ja) | 2021-06-02 |
Family
ID=55862718
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2015094323A Pending JP2016212193A (ja) | 2015-05-01 | 2015-05-01 | 光機能性膜およびその製造方法 |
JP2017551125A Active JP6879929B2 (ja) | 2015-05-01 | 2016-04-13 | 光機能性膜およびその製造方法 |
Family Applications Before (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2015094323A Pending JP2016212193A (ja) | 2015-05-01 | 2015-05-01 | 光機能性膜およびその製造方法 |
Country Status (8)
Country | Link |
---|---|
US (1) | US10859733B2 (ja) |
EP (1) | EP3289394B1 (ja) |
JP (2) | JP2016212193A (ja) |
KR (1) | KR102609050B1 (ja) |
CN (2) | CN107548467A (ja) |
SG (1) | SG11201707494RA (ja) |
TW (1) | TWI772259B (ja) |
WO (1) | WO2016177448A1 (ja) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108878674A (zh) | 2017-05-11 | 2018-11-23 | 京东方科技集团股份有限公司 | 显示基板及其制作方法、显示装置 |
CN108388041B (zh) * | 2018-02-08 | 2021-06-01 | Tcl华星光电技术有限公司 | 彩膜基板及其制造方法、遮光材料及遮光层的制造方法 |
JP7246238B2 (ja) * | 2019-04-18 | 2023-03-27 | リンテック株式会社 | ダイボンド材、発光装置、及び、発光装置の製造方法 |
CN114122157B (zh) * | 2022-01-28 | 2022-05-20 | 浙江晶科能源有限公司 | 光伏电池及其制造方法、光伏组件 |
CN114620947B (zh) * | 2022-03-10 | 2023-03-17 | 福耀玻璃工业集团股份有限公司 | 车辆用憎水减反玻璃及其制造方法与夹层玻璃 |
Family Cites Families (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0856002A (ja) | 1994-08-12 | 1996-02-27 | Sony Corp | ダイオード |
JP4297296B2 (ja) | 1998-09-07 | 2009-07-15 | 大日本印刷株式会社 | 光学機能性膜の製造方法 |
US6805903B2 (en) * | 2000-08-29 | 2004-10-19 | Japan Science And Technology Corporation | Method of forming optical thin film |
JP2005277181A (ja) * | 2004-03-25 | 2005-10-06 | Sharp Corp | 半導体装置の製造方法 |
KR20070017040A (ko) * | 2005-08-03 | 2007-02-08 | 후지필름 홀딩스 가부시끼가이샤 | 반사방지 필름, 편광판 및 영상 표시 장치 |
US8007878B2 (en) * | 2005-08-03 | 2011-08-30 | Fujifilm Corporation | Antireflection film, polarizing plate, and image display device |
JP2007052345A (ja) | 2005-08-19 | 2007-03-01 | Oji Paper Co Ltd | 屈折率傾斜多層薄膜構造体及びその製造方法 |
FR2896887B1 (fr) * | 2006-02-02 | 2008-05-30 | Essilor Int | Article comportant un revetement mesoporeux presentant un profil d'indice de refraction et ses procedes de fabrication |
MY157487A (en) * | 2008-10-17 | 2016-06-15 | Hitachi Chemical Co Ltd | Film having low refractive index film and method for producing the same, anti-reflection film and method for producing the same, coating liquid set for low refractive index film, substrate having microparticle-laminated thin film and method for producing the same, and optical member |
KR101657729B1 (ko) | 2009-01-08 | 2016-09-19 | 나노그램 코포레이션 | 폴리실록산 중합체와 무기 나노입자의 복합체 |
KR20110032820A (ko) * | 2009-09-24 | 2011-03-30 | 서울대학교산학협력단 | 나노입자-고분자 혼성체의 제조방법 및 이러한 방법에 의해 제조된 나노입자-고분자 혼성체 |
JP5810504B2 (ja) * | 2010-10-18 | 2015-11-11 | Jnc株式会社 | 積層体およびその製造方法 |
JP2012181293A (ja) | 2011-02-28 | 2012-09-20 | Fujifilm Corp | 反射防止膜の製造方法 |
JP6004201B2 (ja) | 2011-11-08 | 2016-10-05 | 日産化学工業株式会社 | シラノール基含有ポリシロキサン溶液の安定化方法及び安定化シラノール基含有ポリシロキサン溶液の製造方法 |
JP6000839B2 (ja) | 2012-12-21 | 2016-10-05 | メルクパフォーマンスマテリアルズマニュファクチャリング合同会社 | ケイ素酸化物ナノ粒子とシルセスキオキサンポリマーとの複合体およびその製造方法、ならびにその複合体を用いて製造した複合材料 |
JP6038637B2 (ja) | 2012-12-21 | 2016-12-07 | メルクパフォーマンスマテリアルズマニュファクチャリング合同会社 | 金属酸化物ナノ粒子とシルセスキオキサンポリマーとの複合体およびその製造方法、ならびにその複合体を用いて製造した複合材料 |
WO2015002743A1 (en) * | 2013-07-05 | 2015-01-08 | Gtat Corporation | Polysilazane coating for photovoltaic cells |
TWI632200B (zh) * | 2015-11-26 | 2018-08-11 | 奇美實業股份有限公司 | 感光性聚矽氧烷組成物、保護膜以及具有保護膜的元件 |
EP3597710B1 (en) * | 2018-07-18 | 2021-08-18 | Inkron OY | Novel polysiloxane compositions and uses thereof |
-
2015
- 2015-05-01 JP JP2015094323A patent/JP2016212193A/ja active Pending
-
2016
- 2016-04-13 CN CN201680024603.2A patent/CN107548467A/zh active Pending
- 2016-04-13 KR KR1020177034913A patent/KR102609050B1/ko active IP Right Grant
- 2016-04-13 CN CN202210112735.8A patent/CN114518615A/zh active Pending
- 2016-04-13 WO PCT/EP2016/000608 patent/WO2016177448A1/en active Application Filing
- 2016-04-13 US US15/570,110 patent/US10859733B2/en active Active
- 2016-04-13 SG SG11201707494RA patent/SG11201707494RA/en unknown
- 2016-04-13 EP EP16719769.8A patent/EP3289394B1/en active Active
- 2016-04-13 JP JP2017551125A patent/JP6879929B2/ja active Active
- 2016-04-29 TW TW105113450A patent/TWI772259B/zh active
Also Published As
Publication number | Publication date |
---|---|
SG11201707494RA (en) | 2017-10-30 |
WO2016177448A1 (en) | 2016-11-10 |
JP2018517162A (ja) | 2018-06-28 |
TW201704390A (zh) | 2017-02-01 |
KR102609050B1 (ko) | 2023-12-04 |
US20180149774A1 (en) | 2018-05-31 |
EP3289394B1 (en) | 2024-02-28 |
EP3289394A1 (en) | 2018-03-07 |
KR20180004213A (ko) | 2018-01-10 |
JP2016212193A (ja) | 2016-12-15 |
TWI772259B (zh) | 2022-08-01 |
CN107548467A (zh) | 2018-01-05 |
CN114518615A (zh) | 2022-05-20 |
US10859733B2 (en) | 2020-12-08 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP6879929B2 (ja) | 光機能性膜およびその製造方法 | |
KR101864458B1 (ko) | 저굴절률막 형성용 조성물 및 이것을 사용한 저굴절률막의 형성 방법 | |
KR102092523B1 (ko) | 금속 산화물 나노 입자와 실세스퀴옥산 중합체의 복합체 및 그의 제조 방법, 및 그 복합체를 사용하여 제조한 복합 재료 | |
JP6044792B2 (ja) | 低屈折率膜形成用組成物 | |
JP6360836B2 (ja) | シロキサン化合物を含む反射防止コーティング組成物、それを用いて表面エネルギーが調節された反射防止フィルム | |
JP6430940B2 (ja) | シロキサン化合物を含む反射防止コーティング組成物、これを用いた反射防止フィルム | |
JP6329959B2 (ja) | シロキサン化合物を含む超親水性反射防止コーティング組成物、それを用いた超親水性反射防止フィルムおよびその製造方法 | |
KR20060125770A (ko) | 저굴절률 및 발수성을 갖는 피막 | |
KR20170141703A (ko) | 코팅 조성물 및 광학부재 | |
JP6803842B2 (ja) | オプトエレクトロニクス用途のためのポリシロキサン製剤及びコーティング | |
KR20140134867A (ko) | 저반사특성을 갖는 내오염성 코팅용액 조성물 및 그 제조방법 | |
KR102188211B1 (ko) | 저굴절률막 형성용 조성물 및 그 제조 방법 그리고 저굴절률막의 형성 방법 | |
KR102596586B1 (ko) | 피막 형성용 도포액과 그 제조 방법, 및 피막이 형성된 기재의 제조 방법 | |
JP5310549B2 (ja) | 低屈折率被膜形成用塗布液、その製造方法及び反射防止材 | |
TWI826963B (zh) | 可固化樹脂組成物、薄膜以及顏色轉換面板及顯示裝置 | |
JP7195463B1 (ja) | 熱硬化性樹脂組成物 | |
EP2937319B1 (en) | Method of manufacturing a composition for forming a thin layer with low refractive index, and method of manufacturing a thin layer with low refractive index | |
KR20160096496A (ko) | 투과율이 향상되는 코팅제의 제조방법 | |
CN117651745A (zh) | 涂覆用组合物 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20171002 |
|
AA64 | Notification of invalidation of claim of internal priority (with term) |
Free format text: JAPANESE INTERMEDIATE CODE: A241764 Effective date: 20180306 |
|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20181105 |
|
A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20190905 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20190927 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20191211 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20200228 |
|
A711 | Notification of change in applicant |
Free format text: JAPANESE INTERMEDIATE CODE: A712 Effective date: 20200228 |
|
A711 | Notification of change in applicant |
Free format text: JAPANESE INTERMEDIATE CODE: A711 Effective date: 20200706 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20200827 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20200904 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20201126 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20210402 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20210430 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 6879929 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |