JPH04110918A - Optical component - Google Patents
Optical componentInfo
- Publication number
- JPH04110918A JPH04110918A JP2231222A JP23122290A JPH04110918A JP H04110918 A JPH04110918 A JP H04110918A JP 2231222 A JP2231222 A JP 2231222A JP 23122290 A JP23122290 A JP 23122290A JP H04110918 A JPH04110918 A JP H04110918A
- Authority
- JP
- Japan
- Prior art keywords
- group
- film
- cured film
- fine particles
- titanium oxide
- 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.)
- Pending
Links
- 230000003287 optical effect Effects 0.000 title claims description 26
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000008199 coating composition Substances 0.000 claims abstract description 11
- 125000002252 acyl group Chemical group 0.000 claims abstract description 8
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 8
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 8
- -1 methacryloxy group Chemical group 0.000 claims abstract description 6
- 125000003342 alkenyl group Chemical group 0.000 claims abstract description 4
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 4
- 125000003277 amino group Chemical group 0.000 claims abstract description 4
- 125000004093 cyano group Chemical group *C#N 0.000 claims abstract description 4
- 125000003700 epoxy group Chemical group 0.000 claims abstract description 4
- 125000005843 halogen group Chemical group 0.000 claims abstract description 4
- 125000000962 organic group Chemical group 0.000 claims abstract description 4
- 125000003396 thiol group Chemical group [H]S* 0.000 claims abstract description 4
- 239000010419 fine particle Substances 0.000 claims description 25
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 14
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 12
- 125000003118 aryl group Chemical group 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 150000003377 silicon compounds Chemical class 0.000 abstract description 4
- 230000007062 hydrolysis Effects 0.000 abstract 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052684 Cerium Inorganic materials 0.000 abstract 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 abstract 1
- 229910052700 potassium Inorganic materials 0.000 abstract 1
- 239000011591 potassium Substances 0.000 abstract 1
- 230000035939 shock Effects 0.000 abstract 1
- 239000004033 plastic Substances 0.000 description 24
- 229920003023 plastic Polymers 0.000 description 24
- 238000012360 testing method Methods 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 238000007740 vapor deposition Methods 0.000 description 9
- 239000002585 base Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 238000011282 treatment Methods 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 150000003961 organosilicon compounds Chemical class 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000003628 erosive effect Effects 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 4
- 229910052726 zirconium Inorganic materials 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- SYFOAKAXGNMQAX-UHFFFAOYSA-N bis(prop-2-enyl) carbonate;2-(2-hydroxyethoxy)ethanol Chemical compound OCCOCCO.C=CCOC(=O)OCC=C SYFOAKAXGNMQAX-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000008119 colloidal silica Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 2
- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 description 2
- 229920000298 Cellophane Polymers 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- WHGNXNCOTZPEEK-UHFFFAOYSA-N dimethoxy-methyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](C)(OC)CCCOCC1CO1 WHGNXNCOTZPEEK-UHFFFAOYSA-N 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 229910001936 tantalum oxide Inorganic materials 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N thiocyanic acid Chemical compound SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 2
- UDUKMRHNZZLJRB-UHFFFAOYSA-N triethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OCC)(OCC)OCC)CCC2OC21 UDUKMRHNZZLJRB-UHFFFAOYSA-N 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- RTTZISZSHSCFRH-UHFFFAOYSA-N 1,3-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC(CN=C=O)=C1 RTTZISZSHSCFRH-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- XBIUWALDKXACEA-UHFFFAOYSA-N 3-[bis(2,4-dioxopentan-3-yl)alumanyl]pentane-2,4-dione Chemical compound CC(=O)C(C(C)=O)[Al](C(C(C)=O)C(C)=O)C(C(C)=O)C(C)=O XBIUWALDKXACEA-UHFFFAOYSA-N 0.000 description 1
- DOYKFSOCSXVQAN-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propyl 2-methylprop-2-enoate Chemical compound CCO[Si](C)(OCC)CCCOC(=O)C(C)=C DOYKFSOCSXVQAN-UHFFFAOYSA-N 0.000 description 1
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 description 1
- IKYAJDOSWUATPI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propane-1-thiol Chemical compound CO[Si](C)(OC)CCCS IKYAJDOSWUATPI-UHFFFAOYSA-N 0.000 description 1
- LZMNXXQIQIHFGC-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propyl 2-methylprop-2-enoate Chemical compound CO[Si](C)(OC)CCCOC(=O)C(C)=C LZMNXXQIQIHFGC-UHFFFAOYSA-N 0.000 description 1
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 description 1
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 description 1
- PLXLQGPXPXIVKM-UHFFFAOYSA-N 3-chloropropyl(tripropoxy)silane Chemical compound CCCO[Si](CCCCl)(OCCC)OCCC PLXLQGPXPXIVKM-UHFFFAOYSA-N 0.000 description 1
- KNTKCYKJRSMRMZ-UHFFFAOYSA-N 3-chloropropyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)CCCCl KNTKCYKJRSMRMZ-UHFFFAOYSA-N 0.000 description 1
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 description 1
- GBQYMXVQHATSCC-UHFFFAOYSA-N 3-triethoxysilylpropanenitrile Chemical compound CCO[Si](OCC)(OCC)CCC#N GBQYMXVQHATSCC-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- OTCOSAMIXUWQOA-UHFFFAOYSA-N COC(OC)(OC)CO[SiH2]C Chemical compound COC(OC)(OC)CO[SiH2]C OTCOSAMIXUWQOA-UHFFFAOYSA-N 0.000 description 1
- JYFHYPJRHGVZDY-UHFFFAOYSA-N Dibutyl phosphate Chemical compound CCCCOP(O)(=O)OCCCC JYFHYPJRHGVZDY-UHFFFAOYSA-N 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- 239000002879 Lewis base Substances 0.000 description 1
- VKEQBMCRQDSRET-UHFFFAOYSA-N Methylone Chemical compound CNC(C)C(=O)C1=CC=C2OCOC2=C1 VKEQBMCRQDSRET-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910003134 ZrOx Inorganic materials 0.000 description 1
- JOBBTVPTPXRUBP-UHFFFAOYSA-N [3-(3-sulfanylpropanoyloxy)-2,2-bis(3-sulfanylpropanoyloxymethyl)propyl] 3-sulfanylpropanoate Chemical compound SCCC(=O)OCC(COC(=O)CCS)(COC(=O)CCS)COC(=O)CCS JOBBTVPTPXRUBP-UHFFFAOYSA-N 0.000 description 1
- RQVFGTYFBUVGOP-UHFFFAOYSA-N [acetyloxy(dimethyl)silyl] acetate Chemical compound CC(=O)O[Si](C)(C)OC(C)=O RQVFGTYFBUVGOP-UHFFFAOYSA-N 0.000 description 1
- NOZAQBYNLKNDRT-UHFFFAOYSA-N [diacetyloxy(ethenyl)silyl] acetate Chemical compound CC(=O)O[Si](OC(C)=O)(OC(C)=O)C=C NOZAQBYNLKNDRT-UHFFFAOYSA-N 0.000 description 1
- TVJPBVNWVPUZBM-UHFFFAOYSA-N [diacetyloxy(methyl)silyl] acetate Chemical compound CC(=O)O[Si](C)(OC(C)=O)OC(C)=O TVJPBVNWVPUZBM-UHFFFAOYSA-N 0.000 description 1
- VLFKGWCMFMCFRM-UHFFFAOYSA-N [diacetyloxy(phenyl)silyl] acetate Chemical compound CC(=O)O[Si](OC(C)=O)(OC(C)=O)C1=CC=CC=C1 VLFKGWCMFMCFRM-UHFFFAOYSA-N 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- BJFLSHMHTPAZHO-UHFFFAOYSA-N benzotriazole Chemical compound [CH]1C=CC=C2N=NN=C21 BJFLSHMHTPAZHO-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- SXDBWCPKPHAZSM-UHFFFAOYSA-N bromic acid Chemical compound OBr(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000012975 dibutyltin dilaurate Substances 0.000 description 1
- GENZKBJGWAAVIE-UHFFFAOYSA-N diethoxy-[3-(oxiran-2-ylmethoxy)propyl]-phenylsilane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)CCCOCC1CO1 GENZKBJGWAAVIE-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
- VDCSZEZNBODVRT-UHFFFAOYSA-N dimethoxy-[3-(oxiran-2-ylmethoxy)propyl]-phenylsilane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)CCCOCC1CO1 VDCSZEZNBODVRT-UHFFFAOYSA-N 0.000 description 1
- CVQVSVBUMVSJES-UHFFFAOYSA-N dimethoxy-methyl-phenylsilane Chemical compound CO[Si](C)(OC)C1=CC=CC=C1 CVQVSVBUMVSJES-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- GYLXWHLPLTVIOP-UHFFFAOYSA-N ethenyl(2,2,2-trimethoxyethoxy)silane Chemical compound COC(OC)(OC)CO[SiH2]C=C GYLXWHLPLTVIOP-UHFFFAOYSA-N 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
- ZLNAFSPCNATQPQ-UHFFFAOYSA-N ethenyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C=C ZLNAFSPCNATQPQ-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
- 239000005357 flat glass Substances 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 150000007527 lewis bases Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- RJMRIDVWCWSWFR-UHFFFAOYSA-N methyl(tripropoxy)silane Chemical compound CCCO[Si](C)(OCCC)OCCC RJMRIDVWCWSWFR-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229940082569 selenite Drugs 0.000 description 1
- MCAHWIHFGHIESP-UHFFFAOYSA-L selenite(2-) Chemical compound [O-][Se]([O-])=O MCAHWIHFGHIESP-UHFFFAOYSA-L 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- GYZQBXUDWTVJDF-UHFFFAOYSA-N tributoxy(methyl)silane Chemical compound CCCCO[Si](C)(OCCCC)OCCCC GYZQBXUDWTVJDF-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-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
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- QNKXRZAXBKSFQC-UHFFFAOYSA-N trimethoxy-[3-[2-(oxiran-2-ylmethoxy)ethoxy]propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCCOCC1CO1 QNKXRZAXBKSFQC-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Surface Treatment Of Optical Elements (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、耐擦傷性、密着性、耐衝撃性、透明性に優れ
た光学部品に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an optical component having excellent scratch resistance, adhesion, impact resistance, and transparency.
ジエチレングリコールビスアリルカーボネート樹脂(一
般にCR−39樹脂と呼ばれている)などのプラスチッ
ク基材上に硬化膜を設けた光学部品は良(知られている
。このような硬化膜を設けた光学部品として、例えば特
開昭63−10640号公報には、プラスチックレンズ
上に有機ケイ素化合物とコロイダルシリカとを含むコー
テイング液を塗布硬化して硬化膜を形成してなる光学部
品が、特開昭63−225635号公報にはプラスチッ
クレンズ上に有機ケイ素化合物と酸化チタン微粒子とを
含むコーテイング液を塗布硬化して硬化膜を形成してな
る光学部品が、また特開昭63−223701号公報に
はプラスチックレンズ上にビスシラン化合物、酸化セリ
ウム微粒子、コロイダルシリカとを含むコーテイング液
を塗布硬化して硬化膜を形成してなる光学部品が開示さ
れている。Optical components with a cured film on a plastic base material such as diethylene glycol bisallyl carbonate resin (generally called CR-39 resin) are well known. For example, JP-A No. 63-10640 discloses an optical component in which a coating liquid containing an organosilicon compound and colloidal silica is applied and cured on a plastic lens to form a cured film. The publication describes an optical component in which a coating liquid containing an organosilicon compound and titanium oxide fine particles is coated on a plastic lens and cured to form a cured film, and JP-A-63-223701 discloses an optical component in which a coating liquid containing an organosilicon compound and titanium oxide fine particles is applied and cured to form a cured film. An optical component is disclosed in which a coating liquid containing a bissilane compound, cerium oxide fine particles, and colloidal silica is applied and cured to form a cured film.
特開昭63−10640号公報に開示されている光学部
品は、硬化膜の屈折率が約1.50である。高屈折率プ
ラスチックレンズに前記硬化膜を形成した場合、硬化膜
の屈折率が高屈折率プラスチックレンズの屈折率に比べ
て低いため、干渉縞が認められ、例えば眼鏡レンズとし
て用いるには実用上好ましくない問題点を有している。In the optical component disclosed in JP-A-63-10640, the cured film has a refractive index of about 1.50. When the above-mentioned cured film is formed on a high refractive index plastic lens, since the refractive index of the cured film is lower than that of the high refractive index plastic lens, interference fringes are observed, which is practically preferable for use as an eyeglass lens, for example. It has no problems.
また、特開昭63−225635公報に開示されている
有機ケイ素化合物と酸化チタン微粒子とを含むコーティ
ング組成物から得られた硬化膜は紫外線などの照射によ
り時間とともに酸化チタン微粒子が還元され、青色に着
色する傾向を有し、例えば眼鏡レンズとして使用する場
合にはファッションの面から好ましくない問題点を有し
ている。In addition, a cured film obtained from a coating composition containing an organosilicon compound and titanium oxide fine particles disclosed in JP-A No. 63-225635 turns blue as the titanium oxide fine particles are reduced over time by irradiation with ultraviolet rays. It has a tendency to become colored, which poses a problem that is undesirable from a fashion point of view when it is used, for example, as an eyeglass lens.
また、特開昭63−223701号公報に開示されてい
るビスシラン化合物、酸化セリウム、シリカ微粒子とを
含むコーティング組成物から得られた硬化膜は、耐擦傷
性に劣ると同時に透明性が不十分で、また硬化膜自体が
黄色に着色しやすいため、例えば眼鏡レンズとして使用
する場合には実用上問題がある。Furthermore, a cured film obtained from a coating composition containing a bissilane compound, cerium oxide, and silica fine particles disclosed in JP-A No. 63-223701 has poor scratch resistance and insufficient transparency. Moreover, since the cured film itself tends to be colored yellow, there is a practical problem when using it as an eyeglass lens, for example.
本発明は、かかる問題点を解決するためになされたもの
であり、その目的は耐擦傷性、透明性、耐衝撃性に優れ
、光学部材基板や硬化膜上の反射防止膜との密着性が良
好で、しかも、眼鏡用レンズとして用いた場合でも、干
渉縞等の外観不良が認められにくい新規な光学部品を提
供することにある。The present invention was made to solve these problems, and its purpose is to provide excellent scratch resistance, transparency, and impact resistance, as well as adhesion to optical component substrates and antireflection coatings on cured films. It is an object of the present invention to provide a novel optical component which is of good quality and in which appearance defects such as interference fringes are hard to be observed even when used as a lens for spectacles.
本発明者は、上述の目的を達成するために鋭意研究した
結果、
光学部材上に、
(A)一般式
%式%()
(ここでR1、R1はそれぞれアルキル基、アルケニル
基、アリール基、アシル基または、ハロゲン基、グリシ
ドキシ基、エポキシ基、アミノ基、フェニル基、メルカ
プト基、メタクリオキシ基、あるいは、シアノ基を有す
る有機基、R2は炭素数1〜8のアルキル基、アルコキ
シ基、アシル基、フェニル基、aおよびbは0またはI
である。)で表される有機ケイ素化合物またはその加水
分解物と
(B)酸化セリウム微粒子で被覆された粒径l〜200
ミリミクロンの酸化チタン微粒子と、を含むコーティン
グ組成物を塗布硬化してなる硬化膜を有することを特徴
とする光学部品を見い出し本発明に至った。As a result of intensive research to achieve the above-mentioned object, the present inventors have found that (A) general formula % formula % () (where R1 and R1 are respectively an alkyl group, an alkenyl group, an aryl group, An acyl group, a halogen group, a glycidoxy group, an epoxy group, an amino group, a phenyl group, a mercapto group, a methacryoxy group, or an organic group having a cyano group; R2 is an alkyl group having 1 to 8 carbon atoms, an alkoxy group, an acyl group; group, phenyl group, a and b are 0 or I
It is. ) or a hydrolyzate thereof and (B) a particle size l~200 coated with cerium oxide fine particles.
The present inventors have discovered an optical component characterized by having a cured film formed by coating and curing a coating composition containing millimicron titanium oxide fine particles, resulting in the present invention.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
本発明で(A)成分として用いられる一般式%式%()
(ここでR1、R1はそれぞれアルキル基、アルケニル
基、アリール基、アシル基または、ハロゲン基、グリシ
ドキシ基、エポキシ基、アミノ基、フェニル基、メルカ
プト基、メタクリオキシ基、あるいは、シアノ基を有す
る有機基、R2は炭素数1〜8のアルキル基、アルコキ
シ基、アシル基、フェニル基、aおよびbは口またはI
である。)で表される有機ケイ素化合物またはその加水
分解物の例としては、例えばメチルトリメトキシシラン
、メチルトリエトキシシラン、メチルトリメトキシエト
キシシラン、メチルトリアセトキシシラン、メチルトリ
プロポキシシラン、メチルトリブトキシシラン、エチル
トリメトキシシラン、エチルトリエトキシシラン、ビニ
ルトリメトキシシラン、ビニルトリエトキシシラン、ビ
ニルトリアセトキシシラン、ビニルトリメトキシエトキ
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、フェニルトリアセトキシシラン、γ−
クロロプロピルトリメトキシシラン、γ−クロロプロピ
ルトリエトキシシラン、γ−クロロプロピルトリプロポ
キシシラン、3,3.3−)リフロロプロビルトリメト
キシシラン、γ−グリシドキシプロビルトリメトキシシ
ラン、γ−グリシドキシブロビルトリエトキシシラン、
γ−(βグリシドキシエトキシ)プロピルトリメトキシ
シラン、β−(3,4−エポキシシクロヘキシル)エチ
ルトリメトキシシラン、β−(3,4−エポキシシクロ
ヘキシル)エチルトリエトキシシラン、γ−メタクリル
オキシプロピルトリメトキシシラン、γ−アミノプロピ
ルトリメトキシシラン、γアミノプロピルトリエトキシ
シラン、γ−メルカプトプロピルトリメトキシシラン、
γ−メルカプトプロピルトリエトキシシラン、N−β(
アミノエチル)−γ−アミノプロピルトリメトキシシラ
ン、β−シアノエチルトリエトキシシラン等のトリアル
コキシまたはトリアジルオキシシラン類、およびジメチ
ルジメトキシシラン、フェニルメチルジメトキシシラン
、ジメチルジェトキシシラン、フェニルメチルジェトキ
シシラン、γ−グリシドキシプロピルメチルジメトキシ
シラン、γ−グリシドキシプロビルメチルジェトキシシ
ラン、γ−グリシドキシプロビルフエニルジメトキシシ
ラン、γ−グリシドキシプロビルフエニルジエトキシシ
ラン、γ−クロロプロピルメチルジメトキシシラン、γ
−クロロプロピルメチルジェトキシシラン、ジメチルジ
アセトキシシラン、γ−メタクリルオキシプロピルメチ
ルジメトキシシラン、γ−メタクリルオキシブロピルメ
チルジエトキシシIラン、γ−メルカプトプロピルメチ
ルジメトキシシラン、γ−メルカプトプロピルメチルジ
ェトキシシラン、γ−アミノプロピルメチルジメトキシ
シラン、γアミノプロピルメチルジェトキシシラン、メ
チルビニルジメトキシシラン、メチルビニルジェトキシ
シラン等のジアルコキシシランまたはジアシルオキシシ
ラン類などが挙げられる。The general formula used as component (A) in the present invention is % () (where R1 and R1 are each an alkyl group, an alkenyl group, an aryl group, an acyl group, or a halogen group, a glycidoxy group, an epoxy group, an amino group, An organic group having a phenyl group, a mercapto group, a methacrioxy group, or a cyano group, R2 is an alkyl group having 1 to 8 carbon atoms, an alkoxy group, an acyl group, a phenyl group, a and b are an atom or an I
It is. ) Examples of the organosilicon compounds or their hydrolysates include methyltrimethoxysilane, methyltriethoxysilane, methyltrimethoxyethoxysilane, methyltriacetoxysilane, methyltripropoxysilane, methyltributoxysilane, Ethyltrimethoxysilane, ethyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, vinyltriacetoxysilane, vinyltrimethoxyethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, phenyltriacetoxysilane, γ-
Chloropropyltrimethoxysilane, γ-chloropropyltriethoxysilane, γ-chloropropyltripropoxysilane, 3,3.3-)lifluoroprobyltrimethoxysilane, γ-glycidoxypropyltrimethoxysilane, γ-gly cydoxybrobyltriethoxysilane,
γ-(βglycidoxyethoxy)propyltrimethoxysilane, β-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, β-(3,4-epoxycyclohexyl)ethyltriethoxysilane, γ-methacryloxypropyltri Methoxysilane, γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, γ-mercaptopropyltrimethoxysilane,
γ-Mercaptopropyltriethoxysilane, N-β(
trialkoxy or triazyloxysilanes such as aminoethyl)-γ-aminopropyltrimethoxysilane, β-cyanoethyltriethoxysilane, and dimethyldimethoxysilane, phenylmethyldimethoxysilane, dimethyljethoxysilane, phenylmethyljethoxysilane, γ-glycidoxypropylmethyldimethoxysilane, γ-glycidoxypropylmethyljethoxysilane, γ-glycidoxypropylphenyldimethoxysilane, γ-glycidoxypropylphenyldiethoxysilane, γ-chloro Propylmethyldimethoxysilane, γ
-Chloropropylmethyljethoxysilane, dimethyldiacetoxysilane, γ-methacryloxypropylmethyldimethoxysilane, γ-methacryloxypropylmethyldiethoxysilane, γ-mercaptopropylmethyldimethoxysilane, γ-mercaptopropylmethyljethoxy Examples include dialkoxysilanes or diacyloxysilanes such as silane, γ-aminopropylmethyldimethoxysilane, γ-aminopropylmethyljethoxysilane, methylvinyldimethoxysilane, and methylvinyljethoxysilane.
本発明で(B)成分で用いられる酸化セリウム微粒子で
被覆された粒径l〜200ミリミクロンの酸化チタン微
粒子は、水、有機溶媒またはこれらの混合溶媒に分散さ
せたコロイド溶液の形で用いられ、硬化膜の屈折率、耐
擦傷性を高めるためのものである。酸化セリウム微粒子
で被覆された酸化チタン微粒子を分散させるための有機
溶媒としては、例えばメタノール、エタノール、イソプ
ロピルアルコール等のアルコール類、メチルセロソルブ
、エチルセロソルブ、ブチルセロソルブ等のセロソルブ
類、また、ジメチルホルムアミド等が挙げられる。The titanium oxide fine particles coated with cerium oxide fine particles used as component (B) in the present invention and having a particle size of 1 to 200 millimicrons are used in the form of a colloidal solution dispersed in water, an organic solvent, or a mixed solvent thereof. This is to improve the refractive index and scratch resistance of the cured film. Examples of organic solvents for dispersing titanium oxide fine particles coated with cerium oxide fine particles include alcohols such as methanol, ethanol, and isopropyl alcohol, cellosolves such as methyl cellosolve, ethyl cellosolve, and butyl cellosolve, and dimethyl formamide. Can be mentioned.
酸化チタン微粒子の粒径は1〜200ミリミクロン、特
に好ましくは5〜50ミリミクロンである。粒子径が1
ミリミクロンより小さいものは微粒子の安定性に欠け、
200ミリミクロンを超える粒子径では硬化膜の透明性
に欠けるといった問題点があり好ましくない。The particle size of the titanium oxide fine particles is 1 to 200 millimicrons, particularly preferably 5 to 50 millimicrons. Particle size is 1
Particles smaller than millimicrons lack stability;
Particle diameters exceeding 200 millimicrons are undesirable since there is a problem that the cured film lacks transparency.
酸化セリウム微粒子で被覆された酸化チタンの使用量は
酸化セリウム微粒子で被覆された酸化チタン微粒子の固
形分量/有機ケイ素化合物またはその加水分解物の使用
量の比率が1150〜lO/1となるのが好ましい。比
率がl150では硬化膜の屈折率が低くなり、添加の効
果が小さい。The amount of titanium oxide coated with cerium oxide fine particles is such that the ratio of solid content of titanium oxide fine particles coated with cerium oxide fine particles/amount of organosilicon compound or its hydrolyzate used is 1150 to 1O/1. preferable. When the ratio is l150, the refractive index of the cured film becomes low and the effect of addition is small.
また、10/1を超えると硬化膜と基板の間にクラック
が生じやすくなり、さらに、透明性の低下をきたす可能
性が大きくなる。Moreover, if it exceeds 10/1, cracks are likely to occur between the cured film and the substrate, and furthermore, there is a greater possibility that transparency will be lowered.
本発明で用いられるコーティング組成物は、反応を促進
し、低温で硬化させるために硬化剤を用いることも可能
である。硬化剤としては、例えば、アリルアミン、エチ
ルアミン等のアミン類、またはルイス酸やルイス塩基を
含む各種酸や塩基、例えば、有機カルボン酸、クロム酸
、次亜塩素酸、ホウ酸、臭素酸、亜セレン酸、チオ硫酸
、オルトケイ酸、チオシアン酸、亜硝酸、アルミン酸、
炭酸、過塩素酸等の金属塩、さらにアルミニウム、ジル
コニウム、チタニウム等のアルコキシド又は、これらの
錯化合物などが挙げられる。It is also possible to use a curing agent in the coating composition used in the present invention to accelerate the reaction and cure it at low temperatures. Examples of curing agents include amines such as allylamine and ethylamine, or various acids and bases including Lewis acids and bases, such as organic carboxylic acids, chromic acid, hypochlorous acid, boric acid, bromic acid, and selenite. acids, thiosulfuric acid, orthosilicic acid, thiocyanic acid, nitrous acid, aluminic acid,
Examples include metal salts such as carbonic acid and perchloric acid, alkoxides such as aluminum, zirconium, and titanium, and complex compounds thereof.
又、本発明で用いられるコーティング組成物は基板とな
る光学部材との屈折率を合わせるために、また耐擦傷性
をさらに向上させるために、アルミニウム、アンチモン
、ジルコニウム、スズ、タングテン、ケイ素等の金属酸
化物からなる微粒子状無機物を添加してもよい。In addition, the coating composition used in the present invention is coated with metals such as aluminum, antimony, zirconium, tin, tungsten, and silicon in order to match the refractive index with the optical member serving as the substrate and to further improve scratch resistance. A particulate inorganic substance consisting of an oxide may be added.
本発明で用いるコーティング組成物は塗布時における濡
れ性を向上させ、硬化膜の平滑性を向上させる目的で各
種界面活性剤を添加させることができる。また、紫外線
吸収剤、酸化防止M等も硬化膜の物性に影響を与えない
限り使用可能である。Various surfactants can be added to the coating composition used in the present invention for the purpose of improving wettability during application and improving smoothness of the cured film. Further, ultraviolet absorbers, antioxidant M, etc. can also be used as long as they do not affect the physical properties of the cured film.
塗布手段としてはディッピング法、スピン法、スプレー
法等通常行われる方法が適用できるが、面精度等の面か
ら特にディッピング法、スピン法が好ましい。As the coating means, commonly used methods such as dipping, spinning, and spraying can be used, but dipping and spinning are particularly preferred from the viewpoint of surface precision.
本発明で用いるコーティング組成物の硬化は熱風乾燥、
活性エネルギー線照射によって行うが、好適には、70
℃〜200℃の熱風中で行うのが良(、特に好ましくは
90°C−150℃が望ましい。活性エネルギー線とし
ては遠赤外線等があり熱による損傷を低く抑えることが
できる。The coating composition used in the present invention is cured by hot air drying,
This is carried out by irradiation with active energy rays, preferably 70
It is preferable to carry out in hot air at a temperature of .degree. C. to 200.degree. C. (particularly preferably 90.degree. C. to 150.degree. C.).Active energy rays include far infrared rays, and damage caused by heat can be suppressed to a low level.
さらに、本発明で用いるコーティング組成物を光学部材
基材に塗布する前に、酸、アルカリ、各種有機溶媒によ
る化学処理、プラズマ、紫外線による物理的処理、各種
洗剤による洗浄処理、更には、各種樹脂を用いたプライ
マー処理を行うことによって基材と硬化膜との密着性等
を向上させることができる。Furthermore, before applying the coating composition used in the present invention to the optical member substrate, chemical treatment with acids, alkalis, various organic solvents, physical treatment with plasma and ultraviolet rays, cleaning treatment with various detergents, and furthermore, various resin treatments are performed. The adhesion between the base material and the cured film can be improved by performing the primer treatment using.
本発明により得られた硬化膜を塗布硬化可能な光学部材
としては、透明性を損なうものでなげれば特に限定され
ないが、例としてはメチルメタクリレート単独重合体、
メチルメタクリし一トと1種以上の他のモノマーをモノ
マー成分とする共重合体、ジエチレングリコールビスア
リルカーボネイト単独共重合体、ジエチレングリコール
ビスアリルカーボネートと1種以上の他のモノマーをモ
ノマー成分とする共重合体、ポリカーボネート、ポリス
チレン、ポリ塩化ビニル、ポリエチレンテレフタレート
、ポリウレタン等の合成樹脂、あるいは無機ガラス等が
挙げられる。Optical members that can be coated and cured with the cured film obtained according to the present invention are not particularly limited as long as they do not impair transparency, but examples include methyl methacrylate homopolymer,
Copolymers containing methyl methacrylate and one or more other monomers as monomer components, diethylene glycol bisallyl carbonate homocopolymers, copolymers containing diethylene glycol bisallyl carbonate and one or more other monomers as monomer components Synthetic resins such as synthetic resins, polycarbonate, polystyrene, polyvinyl chloride, polyethylene terephthalate, and polyurethane, and inorganic glasses may be mentioned.
前記硬化膜上に設けられる多層反射防止膜は、低屈折率
と高屈折率とを交互に積層してなり、この時の高屈折率
膜としては、酸化チタン膜、酸化アルミニウム膜、酸化
タンタル膜、酸化ジルコニウム膜等が挙げられるが、透
明性、耐久性等の面からタンタル、ジルコニウム及びイ
ツトリウムを含む金属酸化物の混合蒸着膜を用いたもの
が特に好ましい。なお、低屈折率としては、フッ化マグ
ネシウム膜等が挙げられるが、耐擦傷性、耐熱性等の面
から特に二酸化珪素(Sin2)膜を用いることか特に
好ましい。The multilayer antireflection film provided on the cured film is formed by alternately laminating low refractive index and high refractive index films, and the high refractive index film at this time includes a titanium oxide film, an aluminum oxide film, and a tantalum oxide film. , zirconium oxide film, etc., but from the viewpoint of transparency, durability, etc., a mixed vapor deposited film of metal oxides containing tantalum, zirconium, and yttrium is particularly preferred. In addition, examples of the low refractive index include a magnesium fluoride film, but it is particularly preferable to use a silicon dioxide (Sin2) film from the viewpoint of scratch resistance, heat resistance, and the like.
タンタル、ジルコニウム及びイツトリウムを含む金属酸
化物の混合蒸着膜は、酸化ジルコニウム(ZrCL)粉
末、酸化タンタル(T a 20s )粉末を混合し、
加圧プレス、焼結によりペレット状にしたものを電子ビ
ーム加熱法にて蒸着させたものが好適である。各粉末を
混合してなる混合原料の組成比は、モル比において、Z
r O2が!。A mixed vapor deposition film of metal oxides containing tantalum, zirconium and yttrium is obtained by mixing zirconium oxide (ZrCL) powder and tantalum oxide (T a 20s) powder,
Preferably, the material is made into pellets by pressure pressing and sintering, and then vapor-deposited by electron beam heating. The composition ratio of the mixed raw material obtained by mixing each powder is Z
rO2! .
0に対し、TazOiが0.8〜1.8、y、 。0, TazOi is 0.8 to 1.8, y.
、が0.05〜0.3であることが好ましい。, is preferably 0.05 to 0.3.
このようにして得られる混合金属蒸着膜は、Ta*oh
と同様に、ZrO*に比べ化学的に極めて安定であり
、かつZ r Oxに匹敵する透明性を有している。更
に屈折率において、例えば、2゜05の高い数値を示し
、膜設計上からも有効である。The mixed metal vapor deposited film obtained in this way is Ta*oh
Similarly, it is chemically extremely stable compared to ZrO*, and has transparency comparable to ZrOx. Furthermore, it exhibits a high refractive index of, for example, 2°05, which is effective from the viewpoint of film design.
なお、1モルのZr0zに対して、TazOiが0.8
モル未満の場合や1.8モルを超える場合には、得られ
る混合蒸着膜に吸収膜に吸収が生じ易く、Y*O−が0
.15モル未満では得られる混合蒸着膜に吸収が生じや
すく、0.3モルを超えると、蒸着速度が早くなり、得
られる混合蒸着膜に吸収が生じ易くなるとともに、蒸着
原料の飛散が生じ易くその制御が困難であるため好まし
くない。In addition, TazOi is 0.8 for 1 mol of Zr0z.
If the amount is less than 1.8 mol or more than 1.8 mol, absorption tends to occur in the absorption film in the mixed vapor deposited film obtained, and Y*O- is 0.
.. If it is less than 15 mol, absorption tends to occur in the mixed vapor deposited film obtained, and if it exceeds 0.3 mol, the vapor deposition rate becomes faster and absorption tends to occur in the obtained mixed vapor deposited film, and the vapor deposition raw materials tend to scatter. This is not preferred because it is difficult to control.
多層反射防止膜の膜構成は、λ7′2−λ/4の2層膜
、λ、2′4−λ/4−λ/′4あるいはλ7′4λ/
′2−λ/4の3層膜とすることが実用的には良いが、
反射特性の用途から4層膜以上の多層膜でも可能である
。ここで、3層膜の基板側から数えて第1JIのλ/4
膜は、上記の混合蒸着膜と、SiO2膜を使用した31
1対称等価膜、あるいは2層のコンポジットの等価膜で
あっても良い。The film structure of the multilayer anti-reflection coating is a two-layer film of λ7'2-λ/4, λ, 2'4-λ/4-λ/'4 or λ7'4λ/
Although it is practical to use a three-layer film of '2-λ/4,
A multilayer film of four or more layers is also possible from the viewpoint of reflective properties. Here, λ/4 of the first JI counting from the substrate side of the three-layer film
The film was 31 using the above mixed vapor deposition film and a SiO2 film.
It may be a one-symmetric equivalent film or a two-layer composite equivalent film.
また、多層反射防止膜を成膜するにあたっては上述した
真空蒸着法に代えて、同様の焼結体をターゲット材料と
するスパッタリング法や、イオンブレーティング法等の
方法を用いることもできる。Furthermore, in forming the multilayer anti-reflection film, instead of the above-mentioned vacuum evaporation method, a method such as a sputtering method using a similar sintered body as a target material or an ion-blating method can also be used.
さらに、本発明の光学部品においては、必要に応じて帯
電防止処理、肩先処理等を施すこともできる。Furthermore, the optical component of the present invention may be subjected to antistatic treatment, shoulder treatment, etc., if necessary.
尚、本発明の光学部品は、眼鏡レンズのほか、カメラ用
レンズ、ワードプロセッサーのデイスプレィに付設する
光学フィルター、自動車の窓ガラスなどに使用すること
が可能である。In addition to eyeglass lenses, the optical component of the present invention can be used for camera lenses, optical filters attached to word processor displays, automobile window glasses, and the like.
以下、本発明を実施例により詳細に説明するが、本発明
はこれらの実施例に限定されるものではない。なお、実
施例中の部はすべて重量基準による。EXAMPLES Hereinafter, the present invention will be explained in detail with reference to Examples, but the present invention is not limited to these Examples. Note that all parts in the examples are based on weight.
〔実施例1〕
(プラスチックレンズの作製)
m−キシリレンジイソシアネート100重量部とペンタ
エリスリトールテトラキス3−メルカプトプロピオネー
ト142重量部とリン酸ジ−nブチル6重量部とジブチ
ルスズジラウレート0゜25重量部と紫外線吸収剤とし
て2− (2’ −ヒドロキシ−5° −t−オクチ
ルフェニル)ベンゾトリアゾール0.5重量部を混合し
充分に攪拌したのちlmmHgの真空下で60分脱気を
行った。[Example 1] (Production of plastic lens) 100 parts by weight of m-xylylene diisocyanate, 142 parts by weight of pentaerythritol tetrakis 3-mercaptopropionate, 6 parts by weight of di-n-butyl phosphate, and 0.25 parts by weight of dibutyltin dilaurate. and 0.5 parts by weight of 2-(2'-hydroxy-5°-t-octylphenyl)benzotriazole as an ultraviolet absorber were mixed and thoroughly stirred, followed by deaeration for 60 minutes under a vacuum of lmmHg.
ついで、ガラス製レンズ成形用型と樹脂製ガスケットか
らなる鋳型中に前記混合液を注入し、25°Cから12
0℃まで連続的に20時間かけて昇温し、次いで120
℃2時間保持して重合を行った。重合後ガスケットを除
去し、レンズ成形型とレンズを分離し、プラスチックレ
ンズを得た。Next, the mixed solution was poured into a mold consisting of a glass lens mold and a resin gasket, and heated at 25°C for 12 hours.
The temperature was raised continuously to 0°C over 20 hours, then 120°C.
Polymerization was carried out by holding at °C for 2 hours. After polymerization, the gasket was removed and the lens mold and lens were separated to obtain a plastic lens.
得られたプラスチックレンズはnd=1.592、シd
−36という良好な光学物性を有していた。The obtained plastic lens has nd=1.592, sid
It had good optical properties of -36.
(コーテイング液の調整)
マグネチックスターラーを備えたガラス製の容器に(A
)成分であるγ−グリシドキシプロビルトリメトキシシ
ラン42重量部を加え、攪拌しながら0.01規定塩酸
!4重量部を滴下した。滴下終了後、24時間攪拌を行
い加水分解を物を得た。ついで、(B)成分である酸化
セリウム微粒子で被覆されたメタノール分散酸化チタン
微粒子(固形分2096、平均粒子径15ミリミクロン
)200重量部、溶媒としてイソプロピルアルコール2
0重量部、エチルセロソルブ80重量部、さらに滑剤と
してシリコーン系界面活性剤1重量部、硬化剤としてア
ルミニウムアセチルアセトネート3重量部を加え、充分
に攪拌した後、濾過を行いコーテイング液とした。(Adjustment of coating liquid) In a glass container equipped with a magnetic stirrer (A
) 42 parts by weight of γ-glycidoxypropyltrimethoxysilane was added, and while stirring, 0.01N hydrochloric acid was added! 4 parts by weight was added dropwise. After the dropwise addition was completed, the mixture was stirred for 24 hours to obtain a hydrolyzed product. Next, 200 parts by weight of methanol-dispersed titanium oxide particles (solid content 2096, average particle diameter 15 mm) coated with cerium oxide particles as component (B), and 2 parts by weight of isopropyl alcohol as a solvent were added.
0 parts by weight, 80 parts by weight of ethyl cellosolve, 1 part by weight of a silicone surfactant as a lubricant, and 3 parts by weight of aluminum acetylacetonate as a hardening agent were added, and after thorough stirring, the mixture was filtered to obtain a coating liquid.
(硬化膜の形成)
前記プラスチックレンズ(屈折率nc11.592、ν
d36)を45°Cの5 %N a OH水溶液に3分
間浸漬して充分に洗浄を行った後、上記の方法で調整さ
れたコーテイング液を用いてデイ・ツブ法(引き上げ速
度14 cm/分)でコーティングを行い、120℃で
3時間加熱し硬化膜を形成し、下記評価を行った。(Formation of cured film) The plastic lens (refractive index nc11.592, ν
d36) was immersed in a 5% NaOH aqueous solution at 45°C for 3 minutes to thoroughly wash it, and then coated with the Day-Tub method (pulling speed 14 cm/min) using the coating solution prepared in the above manner. ) and heated at 120° C. for 3 hours to form a cured film, and the following evaluations were performed.
(1)耐擦傷性試験
スチールウール#0000でレンズ表面を擦って傷のつ
きにくさを目視で判断した。判断基準は次のようにした
。(1) Scratch Resistance Test The lens surface was rubbed with #0000 steel wool, and the scratch resistance was visually judged. The judgment criteria were as follows.
A・・・強(擦ってもほとんど傷がつかないB・・・強
く擦るとかなり傷がつく
C・・・レンズ基板と同様の傷がつく
(2)干渉縞の有無
蛍光灯下で目視で判断した。判断基準は次の通りである
。A...Strong (hardly scratched even if rubbed B...severe scratches if rubbed too hard C...scratches similar to the lens board) (2) Presence of interference fringes Visually inspected under fluorescent light The judgment criteria are as follows.
A・・・干渉縞がほとんど見えない
B・・・少し見える
C・・・かなり見える
(3)q!!着性試験
硬化膜付きプラスチックレンズ表面を1mm間隔で10
0目クロスカツトし、セロファンテープを強く貼りつけ
た後、急速に剥がして硬化膜の有無を肩べ、剥離しない
ものを○、剥離したものを×とした。A... Interference fringes are hardly visible B... A little visible C... Quite visible (3) q! ! Adhesion test The surface of a plastic lens with a cured film was 10 mm apart at 1 mm intervals.
A cross cut was made at 0, and a cellophane tape was firmly attached, and then rapidly peeled off to check the presence or absence of a cured film. Those that did not peel were rated as ○, and those that peeled were rated as ×.
(4)耐衝撃性試験
中心厚が1.6m+の平板を用いて、この平板の中心に
127anの高さから16 gI1球を落下させる、F
DA規格に基づく鋼球落下試験を行い、レンズの破損の
有無を調べ、破損しないものをO1破損したものを×と
した。(4) Impact resistance test Using a flat plate with a center thickness of 1.6 m+, drop a 16 gI1 ball from a height of 127 an into the center of the flat plate, F
A steel ball drop test based on the DA standard was conducted to examine the presence or absence of damage to the lens. Those that were not damaged were rated O1, and those that were damaged were rated X.
(5)透明性試験
暗室内、蛍光灯下でレンズに曇りがあるかどうか目視で
肩べた。判断基準は次の通りである。(5) Transparency test In a dark room under fluorescent light, the lenses were visually inspected to see if they were cloudy. The criteria for judgment are as follows.
A・・・曇りがほとんど見えない
B・・・少し見える
C・・・かなり見える
本実施例の硬化膜を有するプラスチックレンズは、耐擦
傷性、密着性が良好で干渉縞が見えず、さらに透明性に
も優れたレンズであることが確認された。A: Hardly visible clouding B: Slightly visible C: Quite visible The plastic lens with the cured film of this example has good scratch resistance and adhesion, no visible interference fringes, and is transparent. It was confirmed that this lens also has excellent performance characteristics.
〔実施例2〕
実施例1で用いた(A)成分のγ−グリシドキシプロピ
ルトリメトキシシラン42重量部の代わりに、γ−グリ
シドキシプロピルメチルジメトキシシラン70重量部を
用いた以外はすべて実施例1と同様に行った。評価結果
は表1に示すように、実施例1と同様、耐擦傷性、密着
性、干渉縞、透明性に優れたレンズであることが確認さ
れた。[Example 2] All except that 70 parts by weight of γ-glycidoxypropylmethyldimethoxysilane was used instead of 42 parts by weight of γ-glycidoxypropyltrimethoxysilane used in component (A) in Example 1. The same procedure as in Example 1 was carried out. As shown in Table 1, the evaluation results confirmed that the lens had excellent scratch resistance, adhesion, interference fringes, and transparency, similar to Example 1.
〔実施例3〕
実施例!で用いた(A)成分のγ−グリシドキシプロピ
ルトリメトキシシラン42重量部の代わりに、β−(3
,4エポキシシクロヘキシル)エチルトリエトキシシラ
ン30重量部、メチルトリメトキシシラン12重量部を
用いた以外は、実施例1と同様に行った。評価結果は表
1に示すように、実施例1と同様、耐擦傷性、密着性、
干渉縞、透明性に優れたレンズであることが確認された
。[Example 3] Example! Instead of 42 parts by weight of γ-glycidoxypropyltrimethoxysilane used in component (A), β-(3
, 4epoxycyclohexyl)ethyltriethoxysilane and 12 parts by weight of methyltrimethoxysilane were used. As shown in Table 1, the evaluation results are the same as in Example 1, including scratch resistance, adhesion,
It was confirmed that the lens has excellent interference fringes and transparency.
〔比較例1〕
実施例1で用いた(B)成分の酸化セリウム微粒子で被
覆された酸化チタン微粒子の代わりにメタノール分散コ
ロイダルシリカ(固形分30%、平均粒子径15ミリミ
クロン)135重量部を用いた以外はすべて実施例1と
同様に行った。結果は、表1に示すように干渉縞が発生
し、外観上好ましくないものであった。[Comparative Example 1] 135 parts by weight of methanol-dispersed colloidal silica (solid content 30%, average particle diameter 15 mm) was used instead of the titanium oxide fine particles coated with cerium oxide fine particles of component (B) used in Example 1. Everything was carried out in the same manner as in Example 1 except for using the following. As a result, as shown in Table 1, interference fringes were generated and the appearance was unfavorable.
(以下余白)
表1
〔実施例4〕
実施例1で得られたプラスチックレンズを以下のように
して多層反射防止膜を形成した。(Margin below) Table 1 [Example 4] A multilayer antireflection film was formed on the plastic lens obtained in Example 1 as follows.
(多層反射防止膜の形成)
下地層および低屈折率膜の蒸着原料として、5jO2焼
結体を、また高屈折率膜である混合蒸着膜の蒸着原料と
して、Z r O2粉末、Ta20i粉末およびy2o
、粉末をモル比で1:1.30.2の割合で混合し、プ
レス形成したのち1200℃で焼結してベレット状にし
たものを用い、前述の方法で硬化膜を設けたプラスチッ
クレンズを蒸着槽に入れ、排気しなから85°Cに加熱
し、2 X 10−”Torrまで排気した後、電子ビ
ーム加熱法にて上記蒸着原料を蒸着させて、表2に示す
ように、ケイ素化合物からなる下地層、混合蒸着膜とケ
イ素化合物膜のコンポジット等価膜からなる第1IIの
低屈折率膜、混合蒸着膜からなる1J2層の高屈折率膜
、およびケイ素酸化物からなる第3層の低屈折率膜を順
次成膜してなる膜構成の多層反射防止膜を得た。(Formation of multilayer anti-reflection film) 5JO2 sintered body was used as the vapor deposition raw material for the base layer and the low refractive index film, and ZrO2 powder, Ta20i powder and Y2O powder were used as the vapor deposition raw material for the mixed vapor deposition film which is the high refractive index film.
, the powders were mixed at a molar ratio of 1:1.30.2, pressed, and then sintered at 1200°C to form a pellet, and a plastic lens with a cured film provided by the method described above was made. The mixture was placed in a vapor deposition tank, heated to 85°C without evacuation, and evacuated to 2 x 10-'' Torr.The above vapor deposition raw materials were vapor-deposited using an electron beam heating method to form a silicon compound as shown in Table 2. a base layer consisting of a base layer consisting of a 1J low refractive index film consisting of a composite equivalent film of a mixed vapor deposited film and a silicon compound film, a 1J2 high refractive index film consisting of a mixed vapor deposited film, and a third low refractive index film consisting of a silicon oxide. A multilayer antireflection film having a film structure formed by sequentially depositing refractive index films was obtained.
なお、下地層は、基板との密着性を向上させるものとし
て用いている。Note that the base layer is used to improve adhesion to the substrate.
(以下余白)
表2
*第1層の低屈折率膜は、コンポジ・ソト等価膜である
。(The following is a blank space) Table 2 *The first layer low refractive index film is a composite sotho-equivalent film.
このようにして得た多層反射防止膜付きプラスチックレ
ンズの可視光線の波長域における吸収率の測定結果を表
3に示す。なお、表3における吸収率(96)は、多層
反射防止膜付きプラスチックレンズの380〜780n
m波長域における反射率(R)および透過率(T)を、
U立製作所340型自記分光光度計を用いて測定し、1
00−(R+T)で換算して求めた。Table 3 shows the measurement results of the absorption rate in the visible light wavelength range of the plastic lens with the multilayer antireflection film obtained in this way. In addition, the absorption coefficient (96) in Table 3 is 380 to 780n of the plastic lens with multilayer antireflection coating.
The reflectance (R) and transmittance (T) in the m wavelength range are
Measured using Utate Seisakusho Model 340 self-recording spectrophotometer, 1
It was calculated by converting it into 00-(R+T).
表3から明らかなように、本実施例4で得られた多層反
射防止膜付きプラスチックレンズは、可視光線の全波長
域にわたって低い吸収率を示し、優れた光学的特性を有
していることが確認された。As is clear from Table 3, the plastic lens with the multilayer antireflection film obtained in Example 4 exhibits low absorption over the entire wavelength range of visible light and has excellent optical properties. confirmed.
また、本実施例4で得られた多層反射防止膜付きプラス
チックレンズの外観、視感反射率、耐擦傷性、耐衝撃性
、密着性、耐熱性、耐アルカリ性、耐酸性を測定した結
果を表4に示す。 表4より、本実施例4の多層反射防
止膜付きプラスチックレンズにおいては、いずれの項目
についても良好な結果が得られ、機械的特性および化学
的特性についても優れていることが確認された。In addition, the results of measuring the appearance, luminous reflectance, scratch resistance, impact resistance, adhesion, heat resistance, alkali resistance, and acid resistance of the plastic lens with multilayer antireflection film obtained in Example 4 are shown. 4. From Table 4, it was confirmed that the plastic lens with multilayer antireflection film of Example 4 had good results in all items, and was also excellent in mechanical properties and chemical properties.
表 3
*原料組成比は、多層反射防止膜を構成する高屈折率膜
として用いた混合蒸着膜の原料組成比を表す。Table 3 *Raw material composition ratio represents the raw material composition ratio of the mixed vapor deposited film used as the high refractive index film constituting the multilayer antireflection film.
〔比較例2〕
実施例1で用いた(B)成分の酸化セリウム微粒子で被
覆された酸化チタン微粒子の代わりにメタノール分散の
酸化チタンゾル(固形分2096、平均粒子径20ミリ
ミクロン)150重量部を用いた以外はすべて実施例4
と同様に行った。結果は、屋外暴露試験で青色に着色し
てしまい、外観上好ましくないものであった。[Comparative Example 2] Instead of the titanium oxide fine particles coated with the cerium oxide fine particles of component (B) used in Example 1, 150 parts by weight of methanol-dispersed titanium oxide sol (solid content 2096, average particle size 20 millimicrons) was used. All except those used were those of Example 4.
I did the same thing. As a result, the product was colored blue in the outdoor exposure test, which was unfavorable in terms of appearance.
〔比較例3〕
実施例Iで用いた(B)成分の酸化セリウム微粒子で被
覆された酸化チタン微粒子の代わりに水分散酸化セリウ
ム(固形分30%、平均粒子径5ミリミクロン)100
重量部を用いた以外はすべて実施例4と同様に行った。[Comparative Example 3] Water-dispersed cerium oxide (solid content 30%, average particle size 5 millimicrons) was used instead of the titanium oxide fine particles coated with cerium oxide fine particles of component (B) used in Example I.
The same procedure as in Example 4 was carried out except that parts by weight were used.
結果は、硬化膜が着色し、透明性も不十分なものであっ
た。As a result, the cured film was colored and had insufficient transparency.
なお、表4における外観、視感反射率、耐擦傷性、耐衝
撃性、密着性、耐アルカリ性、耐酸性および屋外暴露の
評価方法は次の方法によって行った。The evaluation methods for appearance, luminous reflectance, scratch resistance, impact resistance, adhesion, alkali resistance, acid resistance, and outdoor exposure in Table 4 were as follows.
(1)外観
蛍光灯を光源とする照明装置を用い、目視にて下記1)
〜4)を満足するか否か観察し、これらすべてを満足す
るを良、いずれかを満足しないものを不良とした。(1) Exterior Visually check the following 1) using a lighting device with a fluorescent lamp as the light source.
- 4) were observed, and those that satisfied all of these were evaluated as good, and those that did not satisfy any of these were evaluated as poor.
I)透明であること
2)表面に不規則性がないこと
3)着色していないこと
4)表面に異物、傷がないこと
(2)視感反射率
日立製作所340型自記分光光度計を用い、380〜7
80nIn波長域の反射率を測定し、この反射率と視感
度曲線とから視感反射率を換算した。I) It must be transparent 2) There should be no irregularity on the surface 3) It must not be colored 4) There should be no foreign matter or scratches on the surface (2) Luminous reflectance Used with Hitachi Model 340 self-recording spectrophotometer , 380-7
The reflectance in the 80 nIn wavelength range was measured, and the luminous reflectance was calculated from this reflectance and the luminous efficiency curve.
(3)耐擦傷性試験
スチールウール#0000で多層反射防止膜表面を擦っ
て、傷の付きにくさを目視で判断した。(3) Scratch Resistance Test The surface of the multilayer antireflection film was rubbed with steel wool #0000, and the scratch resistance was visually judged.
判断基準は以下のようにした。The judgment criteria were as follows.
A・・・強く擦ってもほとんど傷がつかないB・・・強
く擦るとかなり傷がつく
C・・・レンズ基板と同等の傷がつく
(4)耐擦傷性試験
中心厚が1.6mmの平板を用いて、この平板の中心に
127cmの高さから16gの鋼球を落下させる、FD
A規格に基づ(鋼球落下試験を行い、レンズの破損の有
無を肩べ、破損しないものを○、破損したものを×とし
た。A... There is almost no scratch even if you rub it hard B... You get a lot of scratches if you rub it hard C... You get the same scratches as the lens board (4) Scratch resistance test Center thickness is 1.6 mm FD using a flat plate and dropping a 16 g steel ball from a height of 127 cm onto the center of the flat plate.
Based on the A standard (a steel ball drop test was performed, the presence or absence of damage to the lens was checked. Those that were not damaged were rated ○, and those that were damaged were rated ×.
(5)密着性試験
多層反射防止膜付きプラスチックレンズ表面を1mm間
隔で100目クロスカツトし、セロファンテープを強く
貼りつけた後、急速に剥がして、多層反射防止膜、下地
層およびハードコート膜の剥離の有無を調べ、H離しな
いものをO,剥離したものを×とした。(5) Adhesion test The surface of a plastic lens with a multilayer antireflection film is cross-cutted 100 times at 1 mm intervals, and cellophane tape is firmly attached, then rapidly peeled off to remove the multilayer antireflection film, base layer, and hard coat film. The presence or absence of H was examined, and those that did not release were rated O, and those that peeled were rated ×.
(6)耐熱性試験
硬化膜上に蒸着した多層反射防止膜付きプラスチックレ
ンズをオーブンに1時間入れて加熱し、クラックの発生
の有無を調べた。加熱温度は、70℃より始め、5℃づ
つ上げて、クラックが発生する温度により優劣を判定し
た。(6) Heat Resistance Test A plastic lens with a multilayer antireflection film deposited on the cured film was heated in an oven for 1 hour, and the presence or absence of cracks was examined. The heating temperature started at 70°C and was increased in 5°C increments, and superiority or inferiority was determined based on the temperature at which cracks occur.
(7)耐アルカリ性試験
iowt%NaOH水溶液に、多層反射防止膜付きプラ
スチックレンズを24時間浸漬し、多層反射防止膜表面
の浸食状態を観察し、浸食変化無しのものを○、浸食変
化有りのものを×とした。(7) Alkali resistance test A plastic lens with a multilayer antireflection film was immersed in an iowt% NaOH aqueous solution for 24 hours, and the state of erosion on the surface of the multilayer antireflection film was observed. was marked as ×.
(8)耐酸性試験
10ifto6HC1水溶液およびl Owt%Ht
S 04水溶液に、多層反射防止膜付きプラスチックレ
ンズを24時間浸漬し、多層反射防止膜表面の浸食状態
を観察し、浸食変化無しのものを○、浸食変化有りのも
のを×とした。(8) Acid resistance test 10ifto6HC1 aqueous solution and l Owt%Ht
A plastic lens with a multilayer antireflection film was immersed in the S 04 aqueous solution for 24 hours, and the state of erosion on the surface of the multilayer antireflection film was observed. Those with no erosion change were rated ○, and those with erosion change were rated ×.
(9)屋外暴露試験
屋外に1ケ月間暴露放置し、外観上変化の無いものを○
、変化有りのものを×とした。(9) Outdoor exposure test: Leave exposed outdoors for one month, and if there is no change in appearance, ○
, Those with changes were marked as ×.
(以下余白)
〔発明の効果〕
以上述べたように、本発明によれば、酸化セリウムで被
覆された酸化チタン微粒子を用いた硬化膜は、耐擦傷性
、透明性、密着性に優れ、なおかつ、眼鏡用高屈折率プ
ラスチックレンズにコーティングした場合においても、
膜の屈折率が高屈折率プラスチックレンズの屈折率に合
わせることが可能となり干渉縞の発生が認められにくい
光学部品を提供することが可能になった。(The following is a blank space) [Effects of the Invention] As described above, according to the present invention, a cured film using titanium oxide fine particles coated with cerium oxide has excellent scratch resistance, transparency, and adhesion. , even when coated on high refractive index plastic lenses for eyeglasses.
It has become possible to match the refractive index of the film to the refractive index of a high refractive index plastic lens, making it possible to provide an optical component in which interference fringes are less likely to occur.
さらに、反射防止膜を硬化膜上に塗布した場合には、耐
アルカリ性、耐酸性、耐衝撃性が良好な光学部品を得る
ことが可能になった。Furthermore, when an antireflection film is applied on a cured film, it has become possible to obtain an optical component with good alkali resistance, acid resistance, and impact resistance.
Claims (3)
b)(ここでR^1、R^3はそれぞれアルキル基、ア
ルケニル基、アリール基、アシル基、ハロゲン基、グリ
シドキシ基、エポキシ基、アミノ基、フェニル基、メル
カプト基、メタクリオキシ基、あるいは、シアノ基を有
する有機基、R^2は炭素数1〜8のアルキル基、アル
コキシ基、アシル基、フェニル基、aおよびbは0また
は1である。)で表される有機ケイ素化合物またはその
加水分解物と、(B)酸化セリウム微粒子で被覆された
粒径1〜200ミリミクロンの酸化チタン微粒子と、を
含むコーティング組成物を塗布硬化してなる硬化膜を有
することを特徴とする光学部品。(1) On the optical member, (A) General formula (R^1)a(R^3)bSi(OR^2)4-(a+
b) (where R^1 and R^3 are each an alkyl group, an alkenyl group, an aryl group, an acyl group, a halogen group, a glycidoxy group, an epoxy group, an amino group, a phenyl group, a mercapto group, a methacryloxy group, or an organic group having a cyano group, R^2 is an alkyl group having 1 to 8 carbon atoms, an alkoxy group, an acyl group, a phenyl group, a and b are 0 or 1) or a hydrate thereof An optical component characterized by having a cured film formed by coating and curing a coating composition containing a decomposition product and (B) titanium oxide fine particles having a particle size of 1 to 200 millimicrons coated with cerium oxide fine particles.
徴とする請求項1記載の光学部品。(2) The optical component according to claim 1, further comprising a multilayer antireflection film on the cured film.
とする請求項1または請求項2記載の光学部品。(3) The optical component according to claim 1 or 2, wherein the optical member is a lens for spectacles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2231222A JPH04110918A (en) | 1990-08-31 | 1990-08-31 | Optical component |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2231222A JPH04110918A (en) | 1990-08-31 | 1990-08-31 | Optical component |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04110918A true JPH04110918A (en) | 1992-04-13 |
Family
ID=16920234
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2231222A Pending JPH04110918A (en) | 1990-08-31 | 1990-08-31 | Optical component |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04110918A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016138327A (en) * | 2015-01-29 | 2016-08-04 | 日亜化学工業株式会社 | Vapor deposition material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02264902A (en) * | 1989-04-05 | 1990-10-29 | Toray Ind Inc | High-refractive index hard coating film |
| JPH03256002A (en) * | 1990-03-07 | 1991-11-14 | Toray Ind Inc | Article having antireflectivity |
-
1990
- 1990-08-31 JP JP2231222A patent/JPH04110918A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02264902A (en) * | 1989-04-05 | 1990-10-29 | Toray Ind Inc | High-refractive index hard coating film |
| JPH03256002A (en) * | 1990-03-07 | 1991-11-14 | Toray Ind Inc | Article having antireflectivity |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016138327A (en) * | 2015-01-29 | 2016-08-04 | 日亜化学工業株式会社 | Vapor deposition material |
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