JP3893329B2 - Optical member and organic vapor deposition film for optical member - Google Patents
Optical member and organic vapor deposition film for optical member Download PDFInfo
- Publication number
- JP3893329B2 JP3893329B2 JP2002212906A JP2002212906A JP3893329B2 JP 3893329 B2 JP3893329 B2 JP 3893329B2 JP 2002212906 A JP2002212906 A JP 2002212906A JP 2002212906 A JP2002212906 A JP 2002212906A JP 3893329 B2 JP3893329 B2 JP 3893329B2
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- Japan
- Prior art keywords
- film
- carbon atoms
- layer
- group
- optical member
- 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.)
- Expired - Fee Related
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- 238000007740 vapor deposition Methods 0.000 title claims description 44
- 230000003287 optical effect Effects 0.000 title claims description 43
- 125000004432 carbon atom Chemical group C* 0.000 claims description 44
- 238000000151 deposition Methods 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 230000008021 deposition Effects 0.000 claims description 30
- 229920003023 plastic Polymers 0.000 claims description 30
- 239000004033 plastic Substances 0.000 claims description 30
- 239000000758 substrate Substances 0.000 claims description 29
- 150000002430 hydrocarbons Chemical class 0.000 claims description 28
- 150000002894 organic compounds Chemical class 0.000 claims description 26
- 239000007789 gas Substances 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims description 14
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 11
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 150000003377 silicon compounds Chemical class 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 229930195734 saturated hydrocarbon Natural products 0.000 claims description 7
- 239000004215 Carbon black (E152) Substances 0.000 claims description 6
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 6
- 229910001882 dioxygen Inorganic materials 0.000 claims description 6
- 125000004185 ester group Chemical group 0.000 claims description 6
- 125000001033 ether group Chemical group 0.000 claims description 6
- 229930195733 hydrocarbon Natural products 0.000 claims description 6
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 6
- 150000003961 organosilicon compounds Chemical class 0.000 claims description 6
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 6
- 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 claims description 6
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 239000010408 film Substances 0.000 description 106
- 238000000034 method Methods 0.000 description 14
- 239000003513 alkali Substances 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000002834 transmittance Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- -1 amide compounds Chemical class 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 4
- 239000008199 coating composition Substances 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 239000010955 niobium Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
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- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-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
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 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
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 2
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 2
- HNRMPXKDFBEGFZ-UHFFFAOYSA-N 2,2-dimethylbutane Chemical compound CCC(C)(C)C HNRMPXKDFBEGFZ-UHFFFAOYSA-N 0.000 description 2
- ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 2,3-dimethylbutane Chemical compound CC(C)C(C)C ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 0.000 description 2
- VQKFNUFAXTZWDK-UHFFFAOYSA-N 2-Methylfuran Chemical compound CC1=CC=CO1 VQKFNUFAXTZWDK-UHFFFAOYSA-N 0.000 description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- 101000856234 Clostridium acetobutylicum (strain ATCC 824 / DSM 792 / JCM 1419 / LMG 5710 / VKM B-1787) Butyrate-acetoacetate CoA-transferase subunit A Proteins 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 125000002252 acyl group Chemical group 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- NMJJFJNHVMGPGM-UHFFFAOYSA-N butyl formate Chemical compound CCCCOC=O NMJJFJNHVMGPGM-UHFFFAOYSA-N 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-M hexanoate Chemical compound CCCCCC([O-])=O FUZZWVXGSFPDMH-UHFFFAOYSA-M 0.000 description 2
- 229920001519 homopolymer Polymers 0.000 description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 description 2
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- 150000002902 organometallic compounds Chemical class 0.000 description 2
- PGMYKACGEOXYJE-UHFFFAOYSA-N pentyl acetate Chemical compound CCCCCOC(C)=O PGMYKACGEOXYJE-UHFFFAOYSA-N 0.000 description 2
- 238000009832 plasma treatment Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- RBACIKXCRWGCBB-UHFFFAOYSA-N 1,2-Epoxybutane Chemical compound CCC1CO1 RBACIKXCRWGCBB-UHFFFAOYSA-N 0.000 description 1
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 description 1
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical compound C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- XTDQDBVBDLYELW-UHFFFAOYSA-N 2,2,3-trimethylpentane Chemical compound CCC(C)C(C)(C)C XTDQDBVBDLYELW-UHFFFAOYSA-N 0.000 description 1
- HHOSMYBYIHNXNO-UHFFFAOYSA-N 2,2,5-trimethylhexane Chemical compound CC(C)CCC(C)(C)C HHOSMYBYIHNXNO-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- AVMSWPWPYJVYKY-UHFFFAOYSA-N 2-Methylpropyl formate Chemical compound CC(C)COC=O AVMSWPWPYJVYKY-UHFFFAOYSA-N 0.000 description 1
- XQGBQFWJACUVED-UHFFFAOYSA-N 2-[amino(dimethoxy)silyl]oxypropane Chemical compound CC(O[Si](OC)(OC)N)C XQGBQFWJACUVED-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- 229940093475 2-ethoxyethanol Drugs 0.000 description 1
- KYFDXXXNUGBKLT-UHFFFAOYSA-N 2-ethoxyethynyl(dimethyl)silane Chemical compound CCOC#C[SiH](C)C KYFDXXXNUGBKLT-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- ZVGCJDPEKKEYES-UHFFFAOYSA-N 3-trimethylsilylprop-2-yn-1-ol Chemical compound C[Si](C)(C)C#CCO ZVGCJDPEKKEYES-UHFFFAOYSA-N 0.000 description 1
- CPIVYSAVIPTCCX-UHFFFAOYSA-N 4-methylpentan-2-yl acetate Chemical compound CC(C)CC(C)OC(C)=O CPIVYSAVIPTCCX-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- LTPBRCUWZOMYOC-UHFFFAOYSA-N Beryllium oxide Chemical compound O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 description 1
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 1
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 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
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- DHXVGJBLRPWPCS-UHFFFAOYSA-N Tetrahydropyran Chemical compound C1CCOCC1 DHXVGJBLRPWPCS-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
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-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
- 239000006096 absorbing agent Substances 0.000 description 1
- SPEUIVXLLWOEMJ-UHFFFAOYSA-N acetaldehyde dimethyl acetal Natural products COC(C)OC SPEUIVXLLWOEMJ-UHFFFAOYSA-N 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- AOKMFXQCRBQJOP-UHFFFAOYSA-N benzyl trimethylsilyl ether Chemical compound C[Si](C)(C)OCC1=CC=CC=C1 AOKMFXQCRBQJOP-UHFFFAOYSA-N 0.000 description 1
- MRIWRLGWLMRJIW-UHFFFAOYSA-N benzyl(trimethyl)silane Chemical compound C[Si](C)(C)CC1=CC=CC=C1 MRIWRLGWLMRJIW-UHFFFAOYSA-N 0.000 description 1
- QRHCILLLMDEFSD-UHFFFAOYSA-N bis(ethenyl)-dimethylsilane Chemical compound C=C[Si](C)(C)C=C QRHCILLLMDEFSD-UHFFFAOYSA-N 0.000 description 1
- 229940043232 butyl acetate Drugs 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- AONDIGWFVXEZGD-UHFFFAOYSA-N diacetyloxy(methyl)silicon Chemical compound CC(=O)O[Si](C)OC(C)=O AONDIGWFVXEZGD-UHFFFAOYSA-N 0.000 description 1
- FJWRGPWPIXAPBJ-UHFFFAOYSA-N diethyl(dimethyl)silane Chemical compound CC[Si](C)(C)CC FJWRGPWPIXAPBJ-UHFFFAOYSA-N 0.000 description 1
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- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 description 1
- ZBMGMUODZNQAQI-UHFFFAOYSA-N dimethyl(prop-2-enyl)silicon Chemical compound C[Si](C)CC=C ZBMGMUODZNQAQI-UHFFFAOYSA-N 0.000 description 1
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 description 1
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 1
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
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- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- GCSJLQSCSDMKTP-UHFFFAOYSA-N ethenyl(trimethyl)silane Chemical compound C[Si](C)(C)C=C GCSJLQSCSDMKTP-UHFFFAOYSA-N 0.000 description 1
- QDEZCOQKJSRQNN-UHFFFAOYSA-N ethenyl-dimethyl-phenylsilane Chemical compound C=C[Si](C)(C)C1=CC=CC=C1 QDEZCOQKJSRQNN-UHFFFAOYSA-N 0.000 description 1
- JEWCZPTVOYXPGG-UHFFFAOYSA-N ethenyl-ethoxy-dimethylsilane Chemical compound CCO[Si](C)(C)C=C JEWCZPTVOYXPGG-UHFFFAOYSA-N 0.000 description 1
- NUFVQEIPPHHQCK-UHFFFAOYSA-N ethenyl-methoxy-dimethylsilane Chemical compound CO[Si](C)(C)C=C NUFVQEIPPHHQCK-UHFFFAOYSA-N 0.000 description 1
- DRUOQOFQRYFQGB-UHFFFAOYSA-N ethoxy(dimethyl)silicon Chemical compound CCO[Si](C)C DRUOQOFQRYFQGB-UHFFFAOYSA-N 0.000 description 1
- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical compound CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 description 1
- 229940093499 ethyl acetate Drugs 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- UKAJDOBPPOAZSS-UHFFFAOYSA-N ethyl(trimethyl)silane Chemical compound CC[Si](C)(C)C UKAJDOBPPOAZSS-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- GJRQTCIYDGXPES-UHFFFAOYSA-N iso-butyl acetate Natural products CC(C)COC(C)=O GJRQTCIYDGXPES-UHFFFAOYSA-N 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 description 1
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 229940011051 isopropyl acetate Drugs 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-M isovalerate Chemical compound CC(C)CC([O-])=O GWYFCOCPABKNJV-UHFFFAOYSA-M 0.000 description 1
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
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- KNLUHXUFCCNNIB-UHFFFAOYSA-N n-dimethylsilyl-n-methylmethanamine Chemical compound CN(C)[SiH](C)C KNLUHXUFCCNNIB-UHFFFAOYSA-N 0.000 description 1
- 229940094933 n-dodecane Drugs 0.000 description 1
- QJQAMHYHNCADNR-UHFFFAOYSA-N n-methylpropanamide Chemical compound CCC(=O)NC QJQAMHYHNCADNR-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000003960 organic 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
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- PARWUHTVGZSQPD-UHFFFAOYSA-N phenylsilane Chemical compound [SiH3]C1=CC=CC=C1 PARWUHTVGZSQPD-UHFFFAOYSA-N 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization 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
- 229920002578 polythiourethane polymer 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
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
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- 239000010959 steel Substances 0.000 description 1
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- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-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
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- SPHALHRGAQVBKI-UHFFFAOYSA-N trimethoxysilylmethanol Chemical compound CO[Si](CO)(OC)OC SPHALHRGAQVBKI-UHFFFAOYSA-N 0.000 description 1
- UAIFZYSPVVBOPN-UHFFFAOYSA-N trimethyl(prop-1-en-2-yloxy)silane Chemical compound CC(=C)O[Si](C)(C)C UAIFZYSPVVBOPN-UHFFFAOYSA-N 0.000 description 1
- MNMVKGDEKPPREK-UHFFFAOYSA-N trimethyl(prop-2-enoxy)silane Chemical compound C[Si](C)(C)OCC=C MNMVKGDEKPPREK-UHFFFAOYSA-N 0.000 description 1
- HYWCXWRMUZYRPH-UHFFFAOYSA-N trimethyl(prop-2-enyl)silane Chemical compound C[Si](C)(C)CC=C HYWCXWRMUZYRPH-UHFFFAOYSA-N 0.000 description 1
- ZZRPJWCNCLSOLR-UHFFFAOYSA-N trimethyl(prop-2-ynoxy)silane Chemical compound C[Si](C)(C)OCC#C ZZRPJWCNCLSOLR-UHFFFAOYSA-N 0.000 description 1
- WNWMJFBAIXMNOF-UHFFFAOYSA-N trimethyl(propyl)silane Chemical compound CCC[Si](C)(C)C WNWMJFBAIXMNOF-UHFFFAOYSA-N 0.000 description 1
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- QHUNJMXHQHHWQP-UHFFFAOYSA-N trimethylsilyl acetate Chemical compound CC(=O)O[Si](C)(C)C QHUNJMXHQHHWQP-UHFFFAOYSA-N 0.000 description 1
- VFFKJOXNCSJSAQ-UHFFFAOYSA-N trimethylsilyl benzoate Chemical compound C[Si](C)(C)OC(=O)C1=CC=CC=C1 VFFKJOXNCSJSAQ-UHFFFAOYSA-N 0.000 description 1
- TXZMVBJSLYBOMN-UHFFFAOYSA-N trimethylsilylmethyl acetate Chemical compound CC(=O)OC[Si](C)(C)C TXZMVBJSLYBOMN-UHFFFAOYSA-N 0.000 description 1
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- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
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Description
【０００１】
【発明の属する技術分野】
本発明は、プラスチック基材上に反射防止膜を有する光学部材及びかかる光学部材用の有機蒸着膜に関し、特に、視感反射率が小さく、視感透過率が高いという優れた反射防止性を有するだけでなく、光学部材における、耐衝撃性、密着性、耐熱性、耐摩耗性及び耐アルカリ性に優れ、生産性も良好な光学部材に関する。
【０００２】
【従来の技術】
従来から、プラスチック基材に、無機物質を蒸着してなる反射防止膜を設けた光学部材が知られている。かかる光学部材は優れた反射防止性、耐擦傷性を有している。
しかしながら、このような反射防止膜を有する光学部材は、耐衝撃性及び耐熱性が十分ではない。その課題を解決する方法として、例えば、特開昭63-141001号公報に記載されているように、プラスチック基材と反射防止膜との間に有機化合物よりなるプライマ−層を施すことが知られている。
また、特開平8−62401号公報には、有機金属化合物及び／または有機金属化合物に対する酸素ガスの相対的供給量を変化させるプラズマ重合法により、プラスチック基材上に、高屈折率層と低屈折率層との交互積層体からなる反射防止膜を施した光学部材が知られている。
【０００３】
しかしながら、特開昭63-141001号公報の光学部材は、プライマ−液をプラスチック基材に塗布し、加熱して硬化させ、その後に反射防止膜を蒸着するため、プライマ−層の膜厚が、均一にならないことがあった。また、前記プライマ−層に関し、プライマ−層を施すのは大気中であり、反射防止膜を施すのは真空中であるため、反射防止膜とプライマ−層との間に異物が入りやすく、さらに最終製品を作るまでの時間が長いという課題を有していた。
また、特開平8−62401号公報の光学部材は、金属酸化物の蒸着膜からなる反射防止膜を有する光学部材よりも反射率が低く、さらに耐擦傷性も劣るものであった。
【０００４】
本発明は前記の課題を解決するためになされたもので、反射率が小さく、透過率が高いという優れた反射防止性を有するだけでなく、プラスチック基材上における、耐衝撃性、密着性、耐熱性、耐摩耗性及び耐アルカリ性に優れ、生産性も良好な光学部材を提供することを目的とする。
【０００５】
【課題を解決するための手段】
上述した目的は以下の手段により解決された。その手段とは、プラスチック基材と、無機蒸着膜及び有機蒸着膜より構成される多層反射防止膜を有する光学部材であって、前記有機蒸着膜が有機ケイ素化合物と、炭素及び水素を必須成分とするケイ素非含有有機化合物とを蒸着原料とした光学部材である。
【０００６】
【発明の実施の形態】
本発明では、プラスチック基材上に無機蒸着膜及び有機蒸着膜より構成される多層反射防止膜を有することを特徴とする。
無機蒸着膜は、無機酸化物を蒸着原料とし、従来、反射防止膜として用いられている二酸化ケイ素からなる膜、酸化ニオブからなる膜、及び酸化タンタルからなる膜が挙げられる。
【０００７】
次に、本発明では有機蒸着膜が有機ケイ素化合物と、炭素及び水素を必須成分とするケイ素非含有有機化合物とを蒸着原料としたものであることを特徴とし、有機蒸着膜で用いられる有機ケイ素化合物としては、下記一般式（Ｉ）に示さ
れる化合物が用いられる。
X1
｜
X4−Ｓｉ−X2 ・・・（Ｉ）
｜
X3
（X1〜X4は、それぞれ独立に炭素数１〜６の炭化水素基、−ＯＲ1基（R1は炭素数１〜６の炭化水素基）、−ＣＯＯＲ2基（R2は炭素数１〜６の炭化水素基）または、−ＮＲ3 2（Ｒ3は炭素数１〜６の炭化水素基））
前記Ｒ1〜Ｒ3の具体例としては、メチル基、エチル基、プロピル基、イソプロピル基、ブチル基、イソブチル基、ペンチル基、ビニル基、アリル基、フェニル基等が挙げられる。
【０００８】
一般式（I）で表せる具体的な化合物としては、メチルトリメトキシシラン、ジエトキシジメチルシラン、メチルトリエトキシシラン、トリメチルシラノール、ジメチルエトキシシラン、ヒドロキシメチルトリメトキシシラン、メトキシトリメチルシラン、ジメトキシジメチルシラン、テトラメトキシシラン、ジメチルジメチルアミノシラン、ジアセトキシメチルシラン、アリルジメチルシラン、トリメチルビニルシラン、メトキシジメチルビニルシラン、アセトキシトリメチルシラン、トリメトキシビニルシラン、ジエチルジメチルシラン、エチルトリメチルシラン、エトキシトリメチルシラン、エチルトリメトキシシラン、ジメチルアミノトリメトキシシラン、フェニルシラン、ジメチルジビニルシラン、3-ヒドロキシ-1-プロピニルトリメチルシラン、2-プロピニルオキシトリメチルシラン、ジメチルエトキシエチニルシラン、ジアセトキシジメチルシラン、アリルトリメチルシラン、アリルオキシトリメチルシラン、エトキシジメチルビニルシラン、イソプロペノキシトリメチルシラン、アセトキシメチルトリメチルシラン、Ｎ‐メチル-Ｎ‐トリメチルシリルアセトアミド、トリメチルプロピルシラン、ベンジルオキシトリメチルシラン、ベンジルトリメチルシラン、トリメチルシリルベンゾネート、ジメチルフェニルビニルシラン、プロピルトリエトキシシラン、トリプロピルシラン、3-アリルアミノプロピルトリメトキシシランなどの化合物が挙げられる。
【０００９】
本発明における炭素及び水素を必須成分とするケイ素非含有有機化合物としては、次の（ｉ）〜（ｉｖ）に示す化合物が用いられる。
（ｉ）炭素数５〜１２の飽和炭化水素化合物、
（ｉｉ）酸素原子及び／または窒素原子を有する炭素数３〜１２の有機化合物、
（ｉｉｉ）エステル基を有する炭素数３〜１２の有機化合物、
（ｉｖ）エーテル基を有する炭素数３〜１２の有機化合物
尚、これら（ｉ）〜（ｉｖ）に示す有機化合物は単独でもまた２種以上を混合して使用することもできる。
【００１０】
上述の（ｉ）〜（ｉｖ）の具体的化合物としてはそれぞれ以下のものが挙げられる。
（ｉ）炭素数５〜１２の飽和炭化水素化合物の具体例としては、n-ペンタン、n-ヘキサン、n-ヘプタン、n-オクタン、n-ノナン、n-デカン、n-ドデカン、2-メチルペンタン、2,2-ジメチルブタン、2,3-ジメチルブタン、2,2,3-トリメチルペンタン、イソオクタン、2,2,5-トリメチルヘキサンなどの化合物が挙げられる。
（ｉｉ）酸素原子及び／または窒素原子を有する炭素数３〜１２の有機化合物の具体例としては、2-メトキシエタノール、2-エトキシエタノール、1-メトキシ-2-プロパノール、1-エトキシ-2-プロパノールなどのアルコ−ル化合物、N,N-ジメチルホルムアミド、N,N-ジメチルアセトアミド、N-メチルプロピオンアミドなどのアミド化合物、ε-カプロラクタムなどの化合物が挙げられる。
（ｉｉｉ）エステル基を有する炭素数３〜１２の有機化合物の具体例としては、酢酸メチル、酢酸エチル、酢酸プロピル、酢酸イソプロピル、酢酸ブチル、酢酸イソブチル、酢酸sec-ブチル、酢酸ペンチル、酢酸イソペンチル、酢酸sec-ヘキシル、酢酸ビニル、メタクリル酸メチル、ギ酸エチル、ギ酸プロピル、ギ酸ブチル、ギ酸イソブチル、ギ酸ペンチル、プロピオン酸メチルなどの化合物が挙げられる。
（ｉｖ）エーテル基を有する炭素数３〜１２の有機化合物の具体例としては、ジプロピルエーテル、ジイソプロピルエーテル、ジブチルエーテル、ブチルビニルエーテル、1,2-エポキシブタン、ジオキサン、トリオキサン、2-メチルフラン、テトラヒドロフラン、テトラヒドロピラン、1,2-ジメトキシエタン、1,2-ジエトキシエタン、ジエチレングリコールジメチルエーテル、アセタールなどの化合物が挙げられる。
【００１１】
前述した蒸着原料である有機ケイ素化合物と、炭素及び水素を必須成分とし、酸素及び窒素を任意成分とするケイ素非含有有機化合物との割合は、本発明で意図する物性を得る観点から、該有機化合物の流量50sccmに対し、有機ケイ素化合物の流量が50sccm〜500sccmの範囲が好ましい。
【００１２】
本発明において、反射防止膜は無機酸化物を蒸着原料とする無機蒸着膜と、有機化合物を蒸着原料とする有機蒸着膜の膜構成を有するが、有機蒸着膜は、耐衝撃性を向上するとの観点から、基材側に最も近い位置に設けることが好ましく、さらには反射防止膜の最外層にも併せて設けることが特に好ましい。
また、有機蒸着膜の屈折率は1.42〜1.48の範囲であることが好ましい。二酸化ケイ素からなる層と同等の屈折率にすることによって、従来知られている二酸化ケイ素からなる低屈折率層を前記有機蒸着膜に置き換えることができ、耐衝撃性に良好な部材を得ることが可能である。
【００１３】
有機蒸着膜を形成する方法としては、プラズマ法が好ましく用いられる。その理由は、プラズマエネルギーにより励起した粒子は、化学的に活性なエネルギーを持っており、このエネルギーを利用して基板上に有機材料の重合をくり返すことにより、密着性、耐衝撃性に優れた有機膜を形成することが可能となるからである。
プラズマ法においては、酸素ガス、窒素ガス、アルゴンガス及びこれらの混合ガスが用いられる。
酸素ガスは基板との密着性確保及び、耐衝撃性の向上に好適であり、好ましい流量は50sccm〜500sccmの範囲である。窒素ガスは同様に耐衝撃性向上に好適であり、好ましい流量の範囲は同様に50sccm〜500sccmの範囲である。一方、アルゴンガスは屈折率調整に好適であり、好ましい流量は50sccm〜500sccmの範囲である。該プラズマ法では、これらの混合ガスを用いることで、耐衝撃性向上と、屈折率調整を同時に行うことが可能であり特に好ましい。またこれらの混合ガスを用いる場合の好ましい流量は、酸素、アルゴン、窒素共に50sccm〜500sccmである。
プラズマ装置としては、特に制限されないが、例えば図１に示す装置が用いられ、好ましい真空度は、1.5×10-1Pa 〜 5.0×10-3Paである。また、ＲＦ(Radio Frequency)のパワ−は、プラズマ発生RF出力0.5KW〜6.0KW、プラズマ偏向コイル出力0.5A〜10.0Aの範囲であることが好ましい。
【００１４】
本発明においては、多層反射防止膜が有機蒸着膜と無機蒸着膜が交互に積層されており、さらに、無機蒸着膜が酸化ニオブを蒸着原料とした膜と二酸化ケイ素を蒸着原料とした膜を交互に蒸着したものである。具体的には、以下の構成を有する。尚、ここでは第１層がプラスチック基板に最も近い層であり、第１の態様では第７層がプラスチック基板から最も遠い層であり、第２の態様では第５層がプラスチック基板から最も遠い層である。
第１の態様（反射防止膜）
第１層：有機蒸着膜（膜厚：0.01λ〜1.5λ）
第２層：酸化ニオブを蒸着原料とした膜（膜厚：0.01λ〜0.15λ）
第３層：二酸化ケイ素を蒸着原料とした膜（膜厚：0.03λ〜1.5λ）
第４層：酸化ニオブを蒸着原料とした膜（膜厚：0.05λ〜0.25λ）
第５層：二酸化ケイ素を蒸着原料とした膜（膜厚：0.01λ〜0.25λ）
第６層：酸化ニオブを蒸着原料とした膜（膜厚：0.05λ〜0.25λ）
第７層：有機蒸着膜（膜厚：0.15〜0.35λ）
第２の態様（反射防止膜）
第１層：有機蒸着膜（膜厚：0.01λ〜1.5λ）
第２層：酸化ニオブを蒸着原料とした膜（膜厚：0.01λ〜0.15λ）
第３層：二酸化ケイ素を蒸着原料とした膜（膜厚：0.03λ〜0.25λ）
第４層：酸化ニオブを蒸着原料とした膜（膜厚：0.18λ〜0.6λ）
第５層：有機蒸着膜（膜厚：0.15λ〜0.35λ）
【００１５】
また、前記無機蒸着膜が酸化タンタルを蒸着原料とした膜と二酸化ケイ素を蒸着原料とした膜を交互に蒸着したものも本発明の範囲であり、具体的には以下の構成のものである。尚、第１の態様及び第２の態様と同様に、第１層がプラスチック基板に最も近い層であり、第５層がプラスチック基板から最も遠い層である。
第３の態様（反射防止膜）
第１層：有機蒸着膜（膜厚：0.01λ〜1.5λ）
第２層：酸化タンタルを蒸着原料とした膜（膜厚：0.01λ〜0.15λ）
第３層：二酸化ケイ素を蒸着原料とした膜（膜厚：0.03λ〜0.25λ）
第４層：酸化タンタルを蒸着原料とした膜（膜厚：0.18λ〜0.6λ）
第５層：有機ケイ素化合物及び有機非金属化合物を蒸着原料とした有機蒸着膜（膜厚：0.15λ〜0.35λ）
【００１６】
本発明で使用するプラスチック基材の材質は、特に限定されず、例えば、メチルメタクリレ−ト単独重合体、メチルメタクリレ−トと１種以上の他のモノマ−との共重合体、ジエチレングリコ−ルビスアリルカ−ボネ−ト単独重合体、ジエチレングリコ−ルビスアリルカ−ボネ−トと１種以上の他のモノマ−との共重合体、イオウ含有共重合体、ハロゲン含有共重合体、ポリカ−ボネ−ト、ポリスチレン、ポリ塩化ビニル、不飽和ポリエステル、ポリエチレンテレフタレ−ト、ポリウレタン、ポリチオウレタンなどが挙げられる。
【００１７】
本発明の光学部材は、反射防止膜を施す前に、基板表面をプラズマ処理することができる。プラズマ処理を行う理由は、基板表面にＯＨ基を生成させ、基板と薄膜の密着力を向上させるためである。処理条件としては下記の範囲であることが好ましい。
また、本発明の光学部材は、反射防止膜の下に、密着性を向上させるために、下地層として、後述するハイブリッド層形成の際に触媒作用のある金属、例えば、ニッケル（Ｎｉ）、銀（Ａｇ）、白金（Ｐｔ）、ニオブ（Ｎｂ）及びチタニウム（Ｔｉ）から選ばれる少なくとも１種類からなる層を施すことができる。特に好ましい下地層は、より良好な耐衝撃性を付与させるために、ニオブからなる金属層である。
【００１９】
本発明の光学部材は、前記プラスチック基材と前記下地層との間に、硬化被膜を有しても良い。
硬化被膜としては、通常、金属酸化物コロイド粒子と下記一般式（II）
（Ｒ4）a (Ｒ5)bＳｉ（ＯＲ6）4-(a+b) ・・・（II）
（式中、Ｒ4及びＲ5は、それぞれ独立に、炭素数１〜８のアルキル基、炭素数２〜８のアルケニル基、炭素数６〜８のアリール基、炭素数１〜８のアシル基、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、メタクリロキシ基及びシアノ基の中から選ばれる１種の有機基を示し、Ｒ6は炭素数１〜８のアルキル基、炭素数１〜８のアシル基及び炭素数６〜８のフェニル基の中から選ばれる１種の有機基を示し、ａ及びｂは、それぞれ独立に０又は１の整数である）で表される有機ケイ素化合物とからなる組成物が使用される。
【００２０】
前記金属酸化物コロイド粒子としては、例えば、酸化タングステン（ＷＯ3）、酸化亜鉛（ＺｎＯ）、酸化ケイ素（ＳｉＯ2）、酸化アルミニウム（Ａｌ2Ｏ3）、酸化チタニウム（ＴｉＯ2）、酸化ジルコニウム（ＺｒＯ2）、酸化スズ（ＳｎＯ2）、酸化ベリリウム（ＢｅＯ）又は酸化アンチモン（Ｓｂ2Ｏ5）等が挙げられ、単独又は２種以上を併用することができる。
前記硬化被膜を作るコ−ティング液には、従来知られている方法で、液の調整を行うことができる。所望により、硬化触媒を含有させることができ、また塗布時における濡れ性を向上させ、硬化被膜の平滑性を向上させる目的で各種の有機溶剤や界面活性剤を含有させることもできる。さらに、紫外線吸収剤、酸化防止剤、光安定剤、老化防止剤等もコーティング組成物及び硬化被膜の物性に影響を与えない限り添加することができる。
【００２１】
コ−ティング組成物の硬化は、熱風乾燥または活性エネルギー線照射によって行い、硬化条件としては、７０〜２００℃の熱風中にて行うことが好ましく、特には９０〜１５０℃の範囲で行うことが好ましい。なお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。
また、コ−ティング組成物よりなる硬化膜を基材上に形成する方法としては、上述したコ−ティング組成物を基材に塗布する方法が挙げられる。塗布手段としてはディッピング法、スピンコーティング法、スプレー法等の通常行われる方法が適用できるが、面精度の観点からディッピング法、スピンコーティング法が特に好ましい。
【００２２】
【実施例】
以下、実施例により本発明をさらに詳細に説明するが、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、実施例及び比較例において得られた光学部材の物性評価は以下のようにして行った。
（１）視感透過率
プラスチックレンズの視感透過率Ｙは、両面に反射防止膜を有するプラスチックレンズをサンプルとして、日立分光光度計Ｕ−３４１０を用い測定した。
（２）視感反射率
プラスチックレンズの視感反射率Ｚは、両面に反射防止膜を有するプラスチックレンズをサンプルとして、日立分光光度計Ｕ−３４１０を用い測定した。
（３）耐衝撃性
レンズ中心部厚さ（ＣＴ）２．０ｍｍのレンズを作製してＦＤＡ（Food and Drug Administration）で定められているドロップボールテストを行い、レンズが破損するまでのドロップボール重量を測定した。
（４）密着性
プラスチックレンズの表面に剃刀にて１ｍｍ×１ｍｍの升目を１００個作成し、升目上にセロハンテープを貼り、一気にテープをはがし、残った升目の数で評価した。表中、残った升目の数／１００で記載した。
１００／１００は剥離しない目の数が１００個であることを意味する。
【００２３】
（５）耐摩耗性
プラスチックレンズの表面にスチールウールにて１ｋｇｆ／ｃｍ2の荷重をかけ、１０ストローク擦り、表面状態により以下の基準で評価した。
ＵＡ：殆ど傷なし
Ａ：細い傷数本あり
Ｂ：細い傷多数、太い傷数本あり
Ｃ：細い傷多数、太い傷多数あり
Ｄ：殆ど膜がはがれた状態
（６）耐熱性
プラスチックレンズをドライオーブンで６０℃から、５℃づつ上昇させて１時間加熱し、クラックの発生温度を測定した。
（７）耐アルカリ性
プラスチックレンズをＮａＯＨ１０％水溶液に２０℃、１時間浸漬し、表面状態により以下の基準で評価した。
ＵＡ：殆ど変化なし
Ａ：点状に膜のはがれた個所が数個ある状態
Ｂ：点状に膜のはがれた個所が全面にある状態
Ｃ：点状に膜のはがれた個所が全面にあり、面状にはがれた個所が数個ある状態
Ｄ：殆ど全面の膜がはがれた状態
【００２４】
実施例１
ガラス製容器に、コロイダルシリカ（スノ−テックス−４０、日産化学）９０重量部、有機ケイ素化合物のメチルトリメトキシシラン８１．６重量部、γ−グリシドキシプロピルトリメトキシシラン１７６重量部、０．５Ｎ塩酸２．０重量部、酢酸２０重量部、水９０重量部を加えた液を、室温にて８時間攪拌後、室温にて１６時間放置して加水分解溶液を得た。この溶液に、イソプロピルアルコ−ル１２０重量部、ｎ−ブチルアルコ−ル１２０重量部、アルミニウムアセチルアセトン１６重量部、シリコ−ン系界面活性剤０．２重量部、紫外線吸収剤０．１重量部を加え、室温にて８時間攪拌後、室温にて２４時間熟成させコ−ティング液を得た。
アルカリ水溶液で前処理したプラスチック基板（素材：ジエチレングリコ−ルビスアリルカ−ボネ−ト、屈折率１．５０、中心厚２．０ｍｍ、レンズ度数０．００）を、前記コーティング液の中に浸漬させ、浸漬終了後、引き上げ速度２０ｃｍ／分で引き上げたプラスチック基板を１２０℃で２時間加熱して硬化膜（ハードコートＡ層）を形成した。その後、図１に示す装置にて、プラズマ発生RF(Radio Frequency)出力4.5KW、プラズマ偏向コイル出力6.5A、使用ガスとして酸素300sccm、処理時間60secの条件でプラズマ前処理を行った。
次に、ハードコートＡ層の上に、第１表に示した条件で第１層〜第７層からなる反射防止膜を形成して、プラスチックレンズを得た。評価結果を第１表に示す。第１表に示すように、視感反射率が０．８２％、視感透過率９９．０％、耐衝撃性テストのドロップボ−ルの質量は３６ｇ、密着性テストは１００／１００，耐熱性テストは９５℃で、耐摩耗性、耐アルカリ性は『ＵＡ』であった。
なお、表中LS:530（商品名：信越化学工業（株））は、メチルトリメトキシシランを示す。
【００２５】
実施例２〜６
反射防止膜を第１表に示した条件で第１層〜第７層からなる反射防止膜を形成した以外は、実施例１と同様にして光学部材を作成した。その結果を第１表に示す。このようにして得られた光学部材は、実施例１同様、視感反射率、視感透過率、耐衝撃性、密着性、耐摩耗性及び耐アルカリ性に優れたレンズであった。
【００２６】
比較例１
第１表に示すように第１層及び第７層を、実施例１で設けた有機蒸着膜の代わりに、二酸化ケイ素からなる膜を施し、プラズマ前処理を行わなかった以外は、実施例１と同様にして光学部材を製造し、同様の評価を行った。その結果を第１表に示す。耐衝撃性テストにおけるドロップボ−ルの重量は14ｇで耐熱性は７０℃であった。
【００２７】
比較例２
第１表に示すように第１層及び第７層を、実施例１で設けた２成分からなる有機蒸着膜の代わりに、有機ケイ素化合物からなる１成分の有機蒸着膜を施した以外は、実施例１と同様にして光学部材を製造し、同様の評価を行った。その結果を第１表に示す。耐衝撃性テストにおけるドロップボ−ルの重量は14ｇで耐熱性は７０℃であった。
【００２８】
比較例３
第１表に示すように第１層及び第７層を、実施例１で設けた２成分からなる有機蒸着膜の代わりに、ヘキサンからなる１成分の有機蒸着膜を施した以外は、実施例１と同様にして光学部材を製造し、同様の評価を行った。その結果を第１表に示す。耐衝撃性テストにおけるドロップボ−ルの重量は14ｇ、耐熱性は７０℃、耐擦傷性は『Ｂ』で、耐アルカリ性は『Ｂ』であった。
【００２９】
比較例４
第１表に示すように第１層及び第７層を、実施例４で設けた２成分からなる有機蒸着膜の代わりに、酢酸ビニルからなる１成分の有機蒸着膜を施した以外は、実施例１と同様にして光学部材を施した。その結果を第１表に示す。耐衝撃性テストにおけるドロップボ−ルの重量は14ｇ、耐熱性は７０℃、耐擦傷性は『Ｂ』で、耐アルカリ性は『Ｂ』であった。
【００３０】
【表１】
＊２ ＬＳ：５３０；メチルトリメトキシシラン（商品名：信越化学工業（株））
【００３１】
【表２】
【発明の効果】
本発明によれば、耐衝撃性、密着性、耐摩耗性及び耐アルカリ性に優れた光学部材を得ることができる。
【図面の簡単な説明】
【図１】本発明で使用されるプラズマＣＶＤ装置の概略図である。
【符号の説明】
１：プラズマプロセスガス導入口
２：プラズマ発生用ＲＦコイル
３：炭化水素モノマー導入口
４：シリコン系モノマー導入口
５：プラズマ室
６：プラズマ偏光コイル
７：成膜上面用
８：基板保持用ドーム
９：基板
１０：基板回転軸
１１：成膜下面用
１２：排気系へ接続[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an optical member having an antireflection film on a plastic substrate and an organic vapor deposition film for such an optical member, and in particular, has excellent antireflection properties such as low luminous reflectance and high luminous transmittance. In addition, the present invention relates to an optical member that is excellent in impact resistance, adhesion, heat resistance, wear resistance, alkali resistance, and productivity in an optical member.
[0002]
[Prior art]
2. Description of the Related Art Conventionally, there has been known an optical member in which an antireflection film formed by depositing an inorganic substance on a plastic substrate is provided. Such an optical member has excellent antireflection properties and scratch resistance.
However, an optical member having such an antireflection film is not sufficient in impact resistance and heat resistance. As a method for solving the problem, for example, as described in JP-A-63-141001, it is known to apply a primer layer made of an organic compound between a plastic substrate and an antireflection film. ing.
Japanese Patent Laid-Open No. 8-62401 discloses a high refractive index layer and a low refractive index on a plastic substrate by a plasma polymerization method in which the relative supply of oxygen gas to the organometallic compound and / or organometallic compound is changed. There is known an optical member provided with an antireflection film composed of an alternating laminate with a rate layer.
[0003]
However, the optical member disclosed in JP-A-63-141001 is prepared by applying a primer solution to a plastic substrate, curing it by heating, and then depositing an antireflection film. Sometimes it was not uniform. In addition, with respect to the primer layer, since the primer layer is applied in the air and the antireflection film is applied in a vacuum, foreign matter easily enters between the antireflection film and the primer layer. The problem was that it took a long time to make the final product.
Further, the optical member disclosed in JP-A-8-62401 has a lower reflectance and inferior scratch resistance than an optical member having an antireflection film made of a metal oxide vapor deposition film.
[0004]
The present invention was made in order to solve the above-mentioned problems, and has not only excellent antireflection properties such as low reflectance and high transmittance, but also on the plastic substrate, impact resistance, adhesion, An object of the present invention is to provide an optical member that is excellent in heat resistance, wear resistance and alkali resistance, and also has good productivity.
[0005]
[Means for Solving the Problems]
The object described above has been solved by the following means. The means is an optical member having a plastic substrate and a multilayer antireflection film composed of an inorganic vapor deposition film and an organic vapor deposition film, wherein the organic vapor deposition film contains an organic silicon compound, carbon and hydrogen as essential components. This is an optical member using a silicon-free organic compound as a deposition raw material.
[0006]
DETAILED DESCRIPTION OF THE INVENTION
The present invention is characterized by having a multilayer antireflection film composed of an inorganic vapor deposition film and an organic vapor deposition film on a plastic substrate.
Inorganic deposited film, an inorganic oxide as a deposition material, conventionally, a film made of silicon dioxide that is used as an antireflection film, a film made of acid niobium, and include film made of tantalum oxide.
[0007]
Next, in the present invention, the organic deposited film is an organic silicon compound used as an organic deposited film, characterized in that an organic silicon compound and a silicon-free organic compound containing carbon and hydrogen as essential components are used as a deposition material. the compounds are needed use a compound represented by the following general formula (I).
X1
｜
X4-Si-X2 (I)
｜
X3
(X1 to X4 each independently represent a hydrocarbon group having 1 to 6 carbon atoms, -OR 1 group (R 1 is a hydrocarbon group having 1 to 6 carbon atoms), - COOR 2 group (R 2 is 1 to the number of
Specific examples of R 1 to R 3 include methyl group, ethyl group, propyl group, isopropyl group, butyl group, isobutyl group, pentyl group, vinyl group, allyl group, and phenyl group.
[0008]
Specific compounds represented by the general formula (I) include methyltrimethoxysilane, diethoxydimethylsilane, methyltriethoxysilane, trimethylsilanol, dimethylethoxysilane, hydroxymethyltrimethoxysilane, methoxytrimethylsilane, dimethoxydimethylsilane, Tetramethoxysilane, dimethyldimethylaminosilane, diacetoxymethylsilane, allyldimethylsilane, trimethylvinylsilane, methoxydimethylvinylsilane, acetoxytrimethylsilane, trimethoxyvinylsilane, diethyldimethylsilane, ethyltrimethylsilane, ethoxytrimethylsilane, ethyltrimethoxysilane, dimethyl Aminotrimethoxysilane, phenylsilane, dimethyldivinylsilane, 3-hydroxy-1-propynyltrimethyl Silane, 2-propynyloxytrimethylsilane, dimethylethoxyethynylsilane, diacetoxydimethylsilane, allyltrimethylsilane, allyloxytrimethylsilane, ethoxydimethylvinylsilane, isopropenoxytrimethylsilane, acetoxymethyltrimethylsilane, N-methyl-N-trimethylsilyl Examples include compounds such as acetamide, trimethylpropylsilane, benzyloxytrimethylsilane, benzyltrimethylsilane, trimethylsilylbenzoate, dimethylphenylvinylsilane, propyltriethoxysilane, tripropylsilane, and 3-allylaminopropyltrimethoxysilane.
[0009]
The silicon-free organic compound which carbon and hydrogen in the present invention as an essential component, a compound shown in the following (i) ~ (iv) is used.
(I) a saturated hydrocarbon compound having 5 to 12 carbon atoms,
(Ii) an organic compound having 3 to 12 carbon atoms having an oxygen atom and / or a nitrogen atom,
(Iii) an organic compound having 3 to 12 carbon atoms having an ester group,
(Iv) C3-C12 organic compound having an ether group These organic compounds shown in (i) to (iv) can be used alone or in admixture of two or more.
[0010]
Specific examples of the above-mentioned (i) to (iv) include the following.
(I) Specific examples of the saturated hydrocarbon compound having 5 to 12 carbon atoms include n-pentane, n-hexane, n-heptane, n-octane, n-nonane, n-decane, n-dodecane, and 2-methyl. Examples thereof include pentane, 2,2-dimethylbutane, 2,3-dimethylbutane, 2,2,3-trimethylpentane, isooctane, and 2,2,5-trimethylhexane.
(Ii) Specific examples of the organic compound having 3 to 12 carbon atoms having an oxygen atom and / or a nitrogen atom include 2-methoxyethanol, 2-ethoxyethanol, 1-methoxy-2-propanol, 1-ethoxy-2- Examples include alcohol compounds such as propanol, amide compounds such as N, N-dimethylformamide, N, N-dimethylacetamide and N-methylpropionamide, and compounds such as ε-caprolactam.
(Iii) Specific examples of the organic compound having 3 to 12 carbon atoms having an ester group include methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate, isobutyl acetate, sec-butyl acetate, pentyl acetate, isopentyl acetate, Examples include compounds such as sec-hexyl acetate, vinyl acetate, methyl methacrylate, ethyl formate, propyl formate, butyl formate, isobutyl formate, pentyl formate, and methyl propionate.
(Iv) Specific examples of the organic compound having 3 to 12 carbon atoms having an ether group include dipropyl ether, diisopropyl ether, dibutyl ether, butyl vinyl ether, 1,2-epoxybutane, dioxane, trioxane, 2-methylfuran, Examples include tetrahydrofuran, tetrahydropyran, 1,2-dimethoxyethane, 1,2-diethoxyethane, diethylene glycol dimethyl ether, acetal and the like.
[0011]
From the viewpoint of obtaining the physical properties intended in the present invention, the ratio of the aforementioned organic silicon compound, which is a raw material for vapor deposition, to the silicon-free organic compound containing carbon and hydrogen as essential components and oxygen and nitrogen as optional components, The flow rate of the organosilicon compound is preferably in the range of 50 sccm to 500 sccm with respect to the compound flow rate of 50 sccm.
[0012]
In the present invention, the antireflection film has a film configuration of an inorganic vapor deposition film using an inorganic oxide as a vapor deposition raw material and an organic vapor deposition film using an organic compound as a vapor deposition raw material, and the organic vapor deposition film has improved impact resistance. From the viewpoint, it is preferable to provide it at a position closest to the substrate side, and it is particularly preferable to provide it at the outermost layer of the antireflection film.
The refractive index of the organic vapor deposition film is preferably in the range of 1.42 to 1.48. By making the refractive index equivalent to that of the layer made of silicon dioxide, the conventionally known low refractive index layer made of silicon dioxide can be replaced with the organic vapor-deposited film, and a member having good impact resistance can be obtained. Is possible.
[0013]
As a method of forming the organic vapor deposition film, a plasma method is preferably used. The reason is that particles excited by plasma energy have chemically active energy. By using this energy to repeat polymerization of organic material on the substrate, it has excellent adhesion and impact resistance. This is because an organic film can be formed.
In the plasma method, oxygen gas, nitrogen gas, argon gas, and a mixed gas thereof are used.
Oxygen gas is suitable for securing adhesion to the substrate and improving impact resistance, and a preferred flow rate is in the range of 50 sccm to 500 sccm. Nitrogen gas is also suitable for improving impact resistance, and a preferable flow rate range is similarly in the range of 50 sccm to 500 sccm. On the other hand, argon gas is suitable for adjusting the refractive index, and a preferred flow rate is in the range of 50 sccm to 500 sccm. In the plasma method, using these mixed gases is particularly preferable because it is possible to simultaneously improve the impact resistance and adjust the refractive index. Further, when these mixed gases are used, preferred flow rates for oxygen, argon, and nitrogen are 50 sccm to 500 sccm.
Although it does not restrict | limit especially as a plasma apparatus, For example, the apparatus shown in FIG. 1 is used, and a preferable vacuum degree is 1.5 * 10 < -1 > Pa-5.0 * 10 < -3 > Pa. The RF (Radio Frequency) power is preferably in the range of plasma generation RF output 0.5 KW to 6.0 KW and plasma deflection coil output 0.5 A to 10.0 A.
[0014]
In the present invention, a multilayer antireflection film is an organic deposition film and the inorganic deposited film is alternately laminated, further film inorganic vapor-deposited film is a film and silicon dioxide was deposited material niobium oxide as a deposition material alternating Vapor deposited . Specifically, it has the following configuration . Here, the first layer is the layer closest to the plastic substrate, the seventh layer is the layer farthest from the plastic substrate in the first mode, and the fifth layer is the layer farthest from the plastic substrate in the second mode. It is.
First aspect (antireflection film)
First layer: Organic vapor deposition film (film thickness: 0.01λ to 1.5λ)
Second layer: Film using niobium oxide as a deposition material (film thickness: 0.01λ to 0.15λ)
Third layer: Film using silicon dioxide as a deposition material (film thickness: 0.03λ to 1.5λ)
Fourth layer: Film using niobium oxide as a deposition material (film thickness: 0.05λ to 0.25λ)
Fifth layer: Film using silicon dioxide as a deposition material (film thickness: 0.01λ to 0.25λ)
Sixth layer: Film using niobium oxide as a deposition material (film thickness: 0.05λ to 0.25λ)
Seventh layer: Organic vapor deposition film (film thickness: 0.15-0.35λ)
Second aspect (antireflection film)
First layer: Organic vapor deposition film (film thickness: 0.01λ to 1.5λ)
Second layer: Film using niobium oxide as a deposition material (film thickness: 0.01λ to 0.15λ)
Third layer: Film using silicon dioxide as a deposition material (film thickness: 0.03λ to 0.25λ)
Fourth layer: Film using niobium oxide as a deposition material (film thickness: 0.18λ to 0.6λ)
5th layer: Organic vapor deposition film (film thickness: 0.15λ to 0.35λ)
[0015]
In addition, the inorganic vapor deposition film in which a film using tantalum oxide as a vapor deposition material and a film using silicon dioxide as a vapor deposition material are alternately deposited is also within the scope of the present invention, and specifically has the following configuration . As in the first and second aspects, the first layer is the layer closest to the plastic substrate, and the fifth layer is the layer farthest from the plastic substrate.
Third aspect (antireflection film)
First layer: Organic vapor deposition film (film thickness: 0.01λ to 1.5λ)
Second layer: Film using tantalum oxide as a deposition material (film thickness: 0.01λ to 0.15λ)
Third layer: Film using silicon dioxide as a deposition material (film thickness: 0.03λ to 0.25λ)
Fourth layer: Film using tantalum oxide as a deposition material (film thickness: 0.18λ to 0.6λ)
5th layer: Organic vapor deposition film using organic silicon compound and organic nonmetallic compound as vapor deposition raw material (film thickness: 0.15λ to 0.35λ)
[0016]
The material of the plastic substrate used in the present invention is not particularly limited. For example, methyl methacrylate homopolymer, copolymer of methyl methacrylate and one or more other monomers, diethylene glycol Rubisallyl carbonate homopolymer, copolymer of diethylene glycol bisallyl carbonate and one or more other monomers, sulfur-containing copolymer, halogen-containing copolymer, polycarbonate, polystyrene , Polyvinyl chloride, unsaturated polyester, polyethylene terephthalate, polyurethane, polythiourethane and the like.
[0017]
The optical member of the present invention can perform plasma treatment on the substrate surface before applying the antireflection film. The reason for performing the plasma treatment is to generate OH groups on the substrate surface and improve the adhesion between the substrate and the thin film. The treatment conditions are preferably in the following ranges.
In addition, the optical member of the present invention has a catalytic action when forming a hybrid layer, which will be described later, such as nickel (Ni), silver, etc. A layer made of at least one selected from (Ag), platinum (Pt), niobium (Nb), and titanium (Ti) can be applied. A particularly preferable undercoat layer is a metal layer made of niobium in order to give better impact resistance.
[0019]
The optical member of the present invention may have a cured film between the plastic substrate and the base layer.
As the cured coating, usually metal oxide colloidal particles and the following general formula (II)
(R 4 ) a (R 5 ) b Si (OR 6 ) 4- (a + b) (II)
Wherein R 4 and R 5 are each independently an alkyl group having 1 to 8 carbon atoms, an alkenyl group having 2 to 8 carbon atoms, an aryl group having 6 to 8 carbon atoms, or an acyl group having 1 to 8 carbon atoms. , A halogen group, a glycidoxy group, an epoxy group, an amino group, a phenyl group, a mercapto group, a methacryloxy group, and a cyano group, R 6 represents an alkyl group having 1 to 8 carbon atoms, carbon An organic group selected from an acyl group of 1 to 8 and a phenyl group of 6 to 8 carbon atoms, wherein a and b are each independently an integer of 0 or 1) A composition comprising a silicon compound is used.
[0020]
Examples of the metal oxide colloidal particles include tungsten oxide (WO 3 ), zinc oxide (ZnO), silicon oxide (SiO 2 ), aluminum oxide (Al 2 O 3 ), titanium oxide (TiO 2 ), zirconium oxide ( ZrO 2 ), tin oxide (SnO 2 ), beryllium oxide (BeO), or antimony oxide (Sb 2 O 5 ), and the like can be used alone or in combination of two or more.
The coating liquid for forming the cured film can be adjusted by a conventionally known method. If desired, a curing catalyst can be contained, and various organic solvents and surfactants can be contained for the purpose of improving wettability during coating and improving the smoothness of the cured film. Furthermore, ultraviolet absorbers, antioxidants, light stabilizers, anti-aging agents, and the like can be added as long as they do not affect the physical properties of the coating composition and the cured film.
[0021]
Curing of the coating composition is performed by hot air drying or active energy ray irradiation, and the curing condition is preferably performed in hot air at 70 to 200 ° C., particularly 90 to 150 ° C. preferable. Active energy rays include far infrared rays and the like, and damage due to heat can be kept low.
Moreover, the method of apply | coating the coating composition mentioned above to a base material as a method of forming the cured film which consists of a coating composition on a base material is mentioned. As a coating means, a commonly performed method such as a dipping method, a spin coating method, or a spray method can be applied, but a dipping method or a spin coating method is particularly preferable from the viewpoint of surface accuracy.
[0022]
【Example】
EXAMPLES Hereinafter, although an Example demonstrates this invention further in detail, this invention is not limited to these Examples.
In addition, the physical property evaluation of the optical member obtained in the Example and the comparative example was performed as follows.
(1) Luminous transmittance The luminous transmittance Y of a plastic lens was measured using a Hitachi spectrophotometer U-3410 using a plastic lens having antireflection films on both sides as a sample.
(2) Luminous reflectance Z Luminous reflectance Z of a plastic lens was measured using a Hitachi spectrophotometer U-3410 using a plastic lens having an antireflection film on both sides as a sample.
(3) Impact lens The weight of the drop ball until the lens is damaged by producing a lens with a center thickness (CT) of 2.0 mm and conducting a drop ball test defined by FDA (Food and Drug Administration). Was measured.
(4) Adhesive Plastic lens The surface of the plastic lens was made with 100 razors, 100 cells of 1 mm × 1 mm, cellophane tape was applied on the cells, the tape was peeled off at once, and the number of cells remaining was evaluated. In the table, it is indicated by the number of remaining squares / 100.
100/100 means that the number of eyes that do not peel is 100.
[0023]
(5) Abrasion resistance The surface of the plastic lens was subjected to a load of 1 kgf / cm 2 with steel wool, rubbed for 10 strokes, and evaluated according to the following criteria according to the surface condition.
UA: Almost no scratch A: Some thin scratches B: Many thin scratches, some thick scratches C: Many thin scratches, many thick scratches D: Mostly peeled film (6) Dry heat-resistant plastic lens The temperature was raised from 60 ° C. by 5 ° C. in an oven and heated for 1 hour, and the cracking temperature was measured.
(7) The alkali-resistant plastic lens was immersed in a 10% NaOH aqueous solution at 20 ° C. for 1 hour and evaluated according to the following criteria according to the surface condition.
UA: Almost no change A: State where there are several points where the film is peeled off in a dotted manner B: State where the part where the film is peeled off like a dot is on the entire surface C: There are points where the film is peeled off like a dot State D with several points peeled off in a planar state D: State in which almost the entire film has been peeled off
Example 1
In a glass container, 90 parts by weight of colloidal silica (Snotex-40, Nissan Chemical), 81.6 parts by weight of an organosilicon compound, methyltrimethoxysilane, 176 parts by weight of γ-glycidoxypropyltrimethoxysilane, 0. A solution obtained by adding 2.0 parts by weight of 5N hydrochloric acid, 20 parts by weight of acetic acid and 90 parts by weight of water was stirred at room temperature for 8 hours and then allowed to stand at room temperature for 16 hours to obtain a hydrolysis solution. To this solution, 120 parts by weight of isopropyl alcohol, 120 parts by weight of n-butyl alcohol, 16 parts by weight of aluminum acetylacetone, 0.2 part by weight of a silicone-based surfactant and 0.1 part by weight of an ultraviolet absorber are added. The mixture was stirred at room temperature for 8 hours and then aged at room temperature for 24 hours to obtain a coating solution.
A plastic substrate pretreated with an aqueous alkali solution (material: diethylene glycol bisallyl carbonate, refractive index 1.50, center thickness 2.0 mm, lens power 0.00) is immersed in the coating solution, and the immersion is completed. Thereafter, the plastic substrate pulled up at a pulling rate of 20 cm / min was heated at 120 ° C. for 2 hours to form a cured film (hard coat A layer). Thereafter, plasma pretreatment was performed with the apparatus shown in FIG. 1 under the conditions of plasma generation RF (Radio Frequency) output 4.5 KW, plasma deflection coil output 6.5 A, oxygen used 300 sccm, treatment time 60 sec.
Next, an antireflection film comprising the first to seventh layers was formed on the hard coat A layer under the conditions shown in Table 1 to obtain a plastic lens. The evaluation results are shown in Table 1. As shown in Table 1, the luminous reflectance is 0.82%, the luminous transmittance is 99.0%, the mass of the drop ball of the impact resistance test is 36 g, the adhesion test is 100/100, and the heat resistance. The test was 95 ° C., and the wear resistance and alkali resistance were “UA”.
In the table, LS: 530 (trade name: Shin-Etsu Chemical Co., Ltd.) represents methyltrimethoxysilane.
[0025]
Examples 2-6
An optical member was prepared in the same manner as in Example 1 except that the antireflection film was formed of the first to seventh layers under the conditions shown in Table 1. The results are shown in Table 1. The optical member thus obtained was a lens excellent in luminous reflectance, luminous transmittance, impact resistance, adhesion, abrasion resistance and alkali resistance, as in Example 1.
[0026]
Comparative Example 1
As shown in Table 1, Example 1 except that the first layer and the seventh layer were made of silicon dioxide instead of the organic vapor deposition film provided in Example 1 and plasma pretreatment was not performed. The optical member was manufactured in the same manner as described above, and the same evaluation was performed. The results are shown in Table 1. In the impact resistance test, the weight of the drop ball was 14 g and the heat resistance was 70 ° C.
[0027]
Comparative Example 2
As shown in Table 1, the first layer and the seventh layer were subjected to a one-component organic vapor deposition film composed of an organosilicon compound instead of the two component organic vapor deposition film provided in Example 1. An optical member was produced in the same manner as in Example 1, and the same evaluation was performed. The results are shown in Table 1. In the impact resistance test, the weight of the drop ball was 14 g and the heat resistance was 70 ° C.
[0028]
Comparative Example 3
Example 1 except that the first layer and the seventh layer were subjected to a one-component organic vapor deposition film made of hexane instead of the two-component organic vapor deposition film provided in Example 1 as shown in Table 1. The optical member was manufactured in the same manner as in No. 1, and the same evaluation was performed. The results are shown in Table 1. In the impact resistance test, the weight of the drop ball was 14 g, the heat resistance was 70 ° C., the scratch resistance was “B”, and the alkali resistance was “B”.
[0029]
Comparative Example 4
As shown in Table 1, the first layer and the seventh layer were carried out except that a one-component organic vapor deposition film made of vinyl acetate was applied instead of the two-component organic vapor deposition film provided in Example 4. An optical member was applied in the same manner as in Example 1. The results are shown in Table 1. In the impact resistance test, the weight of the drop ball was 14 g, the heat resistance was 70 ° C., the scratch resistance was “B”, and the alkali resistance was “B”.
[0030]
[Table 1]
[0031]
[Table 2]
【The invention's effect】
According to the present invention, an optical member excellent in impact resistance, adhesion, abrasion resistance and alkali resistance can be obtained.
[Brief description of the drawings]
FIG. 1 is a schematic view of a plasma CVD apparatus used in the present invention.
[Explanation of symbols]
1: Plasma process gas introduction port 2: RF coil for plasma generation 3: Hydrocarbon monomer introduction port 4: Silicon monomer introduction port 5: Plasma chamber 6: Plasma polarization coil 7: For film formation upper surface 8: Substrate holding dome 9 : Substrate 10: Substrate rotating shaft 11: For film formation lower surface 12: Connected to exhaust
Claims (13)
第１層：有機蒸着膜（膜厚： 0.01 λ〜 1.5 λ）
第２層：酸化ニオブを蒸着原料とした膜（膜厚： 0.01 λ〜 0.15 λ）
第３層：二酸化ケイ素を蒸着原料とした膜（膜厚： 0.03 λ〜 1.5 λ）
第４層：酸化ニオブを蒸着原料とした膜（膜厚： 0.05 λ〜 0.25 λ）
第５層：二酸化ケイ素を蒸着原料とした膜（膜厚： 0.01 λ〜 0.25 λ）
第６層：酸化ニオブを蒸着原料とした膜（膜厚： 0.05 λ〜 0.25 λ）
第７層：有機蒸着膜（膜厚： 0.15 λ〜 0.35 λ）
前記有機蒸着膜が下記一般式（Ｉ）で示される有機ケイ素化合物と、炭素数５〜１２の飽和炭化水素化合物、酸素原子及び／または窒素原子を有する炭素数３〜１２の有機化合物、エステル基を有する炭素数３〜１２の有機化合物、及びエーテル基を有する炭素数３〜１２の有機化合物から選ばれる少なくとも１種のケイ素非含有有機化合物とを蒸着原料としたものである光学部材。
X1
｜
X4−Si−X2 ・・・（Ｉ）
｜
X3
（ X1 〜 X4 は、それぞれ独立に、炭素数１〜６の炭化水素基、−ＯＲ 1 基（ R 1 は炭素数１〜６の炭化水素基）、−ＣＯＯＲ 2 基（ R 2 は炭素数１〜６の炭化水素基）または、−ＮＲ 3 2 （Ｒ 3 は炭素数１〜６の炭化水素基）） An optical member having a plastic substrate and a multilayer antireflection film composed of the following layers ,
First layer: organic vapor deposition film (thickness: 0.01 λ~ 1.5 λ)
Second layer: has a niobium oxide deposition material film (film thickness: 0.01 λ~ 0.15 λ)
Third layer: film and silicon dioxide deposition material (film thickness: 0.03 λ~ 1.5 λ)
Fourth layer: it was niobium oxide deposition material film (film thickness: 0.05 λ~ 0.25 λ)
Layer 5: film and silicon dioxide deposition material (film thickness: 0.01 λ~ 0.25 λ)
Layer 6: it was a niobium oxide deposition material film (film thickness: 0.05 λ~ 0.25 λ)
Layer 7: organic vapor deposition film (thickness: 0.15 λ~ 0.35 λ)
The organic vapor deposition film is an organosilicon compound represented by the following general formula (I), a saturated hydrocarbon compound having 5 to 12 carbon atoms, an organic compound having 3 to 12 carbon atoms having an oxygen atom and / or a nitrogen atom, an ester group The optical member which uses as a deposition raw material at least 1 sort (s) of silicon-free organic compound chosen from a C3-C12 organic compound which has C3-12, and a C3-C12 organic compound which has ether group .
X1
｜
X4-Si-X2 (I)
｜
X3
( X1 to X4 are each independently a hydrocarbon group having 1 to 6 carbon atoms, —OR 1 group ( R 1 is a hydrocarbon group having 1 to 6 carbon atoms), —COOR 2 group ( R 2 is 1 carbon atom) ˜6 hydrocarbon group) or —NR 3 2 (R 3 is a hydrocarbon group having 1 to 6 carbon atoms))
第１層：有機蒸着膜（膜厚： 0.01 λ〜 1.5 λ）
第２層：酸化ニオブを蒸着原料とした膜（膜厚： 0.01 λ〜 0.15 λ）
第３層：二酸化ケイ素を蒸着原料とした膜（膜厚： 0.03 λ〜 0.25 λ）
第４層：酸化ニオブを蒸着原料とした膜（膜厚： 0.18 λ〜 0.6 λ）
第５層：有機蒸着膜（膜厚： 0.15 λ〜 0.35 λ）
前記有機蒸着膜が下記一般式（Ｉ）で示される有機ケイ素化合物と、炭素数５〜１２の飽和炭化水素化合物、酸素原子及び／または窒素原子を有する炭素数３〜１２の有機化合物、エステル基を有する炭素数３〜１２の有機化合物、及びエーテル基を有する炭素数３〜１２の有機化合物から選ばれる少なくとも１種のケイ素非含有有機化合物とを蒸着原料としたものである光学部材。
X1
｜
X4−Si−X2 ・・・（Ｉ）
｜
X3
（ X1 〜 X4 は、それぞれ独立に、炭素数１〜６の炭化水素基、−ＯＲ 1 基（ R 1 は炭素数１〜６の炭化水素基）、−ＣＯＯＲ 2 基（ R 2 は炭素数１〜６の炭化水素基）または、−ＮＲ 3 2 （Ｒ 3 は炭素数１〜６の炭化水素基）） An optical member having a plastic substrate and a multilayer antireflection film composed of the following layers,
First layer: organic vapor deposition film (thickness: 0.01 λ~ 1.5 λ)
Second layer: has a niobium oxide deposition material film (film thickness: 0.01 λ~ 0.15 λ)
Third layer: film and silicon dioxide deposition material (film thickness: 0.03 λ~ 0.25 λ)
Fourth layer: it was niobium oxide deposition material film (film thickness: 0.18 λ~ 0.6 λ)
Layer 5: organic vapor deposition film (thickness: 0.15 λ~ 0.35 λ)
The organic vapor deposition film is an organosilicon compound represented by the following general formula (I), a saturated hydrocarbon compound having 5 to 12 carbon atoms, an organic compound having 3 to 12 carbon atoms having an oxygen atom and / or a nitrogen atom, an ester group The optical member which uses as a deposition raw material at least 1 sort (s) of silicon-free organic compound chosen from a C3-C12 organic compound which has C3-12, and a C3-C12 organic compound which has ether group.
X1
｜
X4-Si-X2 (I)
｜
X3
( X1 to X4 are each independently a hydrocarbon group having 1 to 6 carbon atoms, —OR 1 group ( R 1 is a hydrocarbon group having 1 to 6 carbon atoms), —COOR 2 group ( R 2 is 1 carbon atom) ˜6 hydrocarbon group) or —NR 3 2 (R 3 is a hydrocarbon group having 1 to 6 carbon atoms))
第１層：有機蒸着膜（膜厚： 0.01 λ〜 1.5 λ）
第２層：酸化タンタルを蒸着原料とした膜（膜厚： 0.01 λ〜 0.15 λ）
第３層：二酸化ケイ素を蒸着原料とした膜（膜厚： 0.03 λ〜 0.25 λ）
第４層：酸化タンタルを蒸着原料とした膜（膜厚： 0.18 λ〜 0.6 λ）
第５層：有機蒸着膜（膜厚： 0.15 λ〜 0.35 λ）
前記有機蒸着膜が下記一般式（Ｉ）で示される有機ケイ素化合物と、炭素数５〜１２の飽和炭化水素化合物、酸素原子及び／または窒素原子を有する炭素数３〜１２の有機化合物、エステル基を有する炭素数３〜１２の有機化合物、及びエーテル基を有する炭素数３〜１２の有機化合物から選ばれる少なくとも１種のケイ素非含有有機化合物とを蒸着原料としたものである光学部材。
X1
｜
X4−Si−X2 ・・・（Ｉ）
｜
X3
（ X1 〜 X4 は、それぞれ独立に、炭素数１〜６の炭化水素基、−ＯＲ 1 基（ R 1 は炭素数１〜６の炭化水素基）、−ＣＯＯＲ 2 基（ R 2 は炭素数１〜６の炭化水素基）または、−ＮＲ 3 2 （Ｒ 3 は炭素数１〜６の炭化水素基）） An optical member having a plastic substrate and a multilayer antireflection film composed of the following layers,
First layer: organic vapor deposition film (thickness: 0.01 λ~ 1.5 λ)
Second layer: has a tantalum oxide deposition material film (film thickness: 0.01 λ~ 0.15 λ)
Third layer: film and silicon dioxide deposition material (film thickness: 0.03 λ~ 0.25 λ)
Fourth layer: it was tantalum oxide deposition material film (film thickness: 0.18 λ~ 0.6 λ)
Layer 5: organic vapor deposition film (thickness: 0.15 λ~ 0.35 λ)
The organic vapor deposition film is an organosilicon compound represented by the following general formula (I), a saturated hydrocarbon compound having 5 to 12 carbon atoms, an organic compound having 3 to 12 carbon atoms having an oxygen atom and / or a nitrogen atom, an ester group The optical member which uses as a deposition raw material at least 1 sort (s) of silicon-free organic compound chosen from a C3-C12 organic compound which has C3-12, and a C3-C12 organic compound which has ether group.
X1
｜
X4-Si-X2 (I)
｜
X3
( X1 to X4 are each independently a hydrocarbon group having 1 to 6 carbon atoms, —OR 1 group ( R 1 is a hydrocarbon group having 1 to 6 carbon atoms), —COOR 2 group ( R 2 is 1 carbon atom) ˜6 hydrocarbon group) or —NR 3 2 (R 3 is a hydrocarbon group having 1 to 6 carbon atoms))
X1
｜
X4−Si−X2 ・・・（Ｉ）
｜
X3
（ X1 〜 X4 は、それぞれ独立に、炭素数１〜６の炭化水素基、−ＯＲ 1 基（ R 1 は炭素数１〜６の炭化水素基）、−ＣＯＯＲ 2 基（ R 2 は炭素数１〜６の炭化水素基）または、−ＮＲ 3 2 （Ｒ 3 は炭素数１〜６の炭化水素基）） In an atmosphere of gas plasma, an organic silicon compound represented by the following general formula (I), a saturated hydrocarbon compound having 5 to 12 carbon atoms, an organic compound having 3 to 12 carbon atoms having an oxygen atom and / or a nitrogen atom, Organic vapor-deposited film for optical members obtained by simultaneously vapor-depositing at least one silicon-free organic compound selected from an organic compound having 3 to 12 carbon atoms having an ester group and an organic compound having 3 to 12 carbon atoms having an ether group .
X1
｜
X4-Si-X2 (I)
｜
X3
( X1 to X4 are each independently a hydrocarbon group having 1 to 6 carbon atoms, —OR 1 group ( R 1 is a hydrocarbon group having 1 to 6 carbon atoms), —COOR 2 group ( R 2 is 1 carbon atom) ˜6 hydrocarbon group) or —NR 3 2 (R 3 is a hydrocarbon group having 1 to 6 carbon atoms))
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002212906A JP3893329B2 (en) | 2002-07-22 | 2002-07-22 | Optical member and organic vapor deposition film for optical member |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002212906A JP3893329B2 (en) | 2002-07-22 | 2002-07-22 | Optical member and organic vapor deposition film for optical member |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2004054048A JP2004054048A (en) | 2004-02-19 |
| JP3893329B2 true JP3893329B2 (en) | 2007-03-14 |
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| JP2002212906A Expired - Fee Related JP3893329B2 (en) | 2002-07-22 | 2002-07-22 | Optical member and organic vapor deposition film for optical member |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4593949B2 (en) * | 2004-03-23 | 2010-12-08 | Ｈｏｙａ株式会社 | Manufacturing method of optical member |
| JP4707656B2 (en) * | 2004-03-29 | 2011-06-22 | Ｈｏｙａ株式会社 | Optical member having antireflection film |
| JP5156251B2 (en) * | 2007-03-30 | 2013-03-06 | Ｈｏｙａ株式会社 | Deposition film evaluation method and spectacle lens manufacturing method using the same |
| EP4289519A1 (en) * | 2022-06-10 | 2023-12-13 | Basf Se | Plasma-created barriers for packaging |
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