JP2021523424A - ホログラム媒体 - Google Patents
ホログラム媒体 Download PDFInfo
- Publication number
- JP2021523424A JP2021523424A JP2021514275A JP2021514275A JP2021523424A JP 2021523424 A JP2021523424 A JP 2021523424A JP 2021514275 A JP2021514275 A JP 2021514275A JP 2021514275 A JP2021514275 A JP 2021514275A JP 2021523424 A JP2021523424 A JP 2021523424A
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- JP
- Japan
- Prior art keywords
- hologram
- polymer
- silane
- functional group
- acrylate
- 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.)
- Granted
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- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 51
- 229920000642 polymer Polymers 0.000 claims abstract description 51
- 230000003287 optical effect Effects 0.000 claims abstract description 30
- 239000002952 polymeric resin Substances 0.000 claims abstract description 16
- 229920003002 synthetic resin Polymers 0.000 claims abstract description 16
- 125000002723 alicyclic group Chemical group 0.000 claims abstract description 11
- 229920002284 Cellulose triacetate Polymers 0.000 claims abstract description 10
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 claims abstract description 10
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 10
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 10
- 229920000098 polyolefin Polymers 0.000 claims abstract description 10
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 87
- 229910000077 silane Inorganic materials 0.000 claims description 83
- 125000000524 functional group Chemical group 0.000 claims description 67
- 239000000463 material Substances 0.000 claims description 40
- 239000000178 monomer Substances 0.000 claims description 40
- 239000003431 cross linking reagent Substances 0.000 claims description 27
- 229920003122 (meth)acrylate-based copolymer Polymers 0.000 claims description 25
- 239000011159 matrix material Substances 0.000 claims description 21
- 150000001875 compounds Chemical class 0.000 claims description 19
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 13
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 13
- 229910052731 fluorine Inorganic materials 0.000 claims description 13
- 239000011737 fluorine Substances 0.000 claims description 13
- 229920000570 polyether Polymers 0.000 claims description 13
- 229920000307 polymer substrate Polymers 0.000 claims description 4
- 125000001033 ether group Chemical group 0.000 claims description 3
- 125000003368 amide group Chemical group 0.000 claims description 2
- 125000004185 ester group Chemical group 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 49
- 238000000034 method Methods 0.000 description 36
- 238000004519 manufacturing process Methods 0.000 description 31
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 30
- 239000000126 substance Substances 0.000 description 20
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 15
- 230000008569 process Effects 0.000 description 15
- 239000000047 product Substances 0.000 description 15
- 125000004432 carbon atom Chemical group C* 0.000 description 14
- 239000010410 layer Substances 0.000 description 14
- 239000003505 polymerization initiator Substances 0.000 description 13
- 238000004132 cross linking Methods 0.000 description 12
- 238000005259 measurement Methods 0.000 description 12
- 125000000217 alkyl group Chemical group 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 230000007423 decrease Effects 0.000 description 10
- 239000003960 organic solvent Substances 0.000 description 10
- 239000000758 substrate Substances 0.000 description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 9
- 239000000975 dye Substances 0.000 description 9
- 229920005862 polyol Polymers 0.000 description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 150000003077 polyols Chemical class 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 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 7
- 239000012948 isocyanate Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 239000004014 plasticizer Substances 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 5
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 5
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 5
- 230000000704 physical effect Effects 0.000 description 5
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 5
- 230000000007 visual effect Effects 0.000 description 5
- VVBLNCFGVYUYGU-UHFFFAOYSA-N 4,4'-Bis(dimethylamino)benzophenone Chemical compound C1=CC(N(C)C)=CC=C1C(=O)C1=CC=C(N(C)C)C=C1 VVBLNCFGVYUYGU-UHFFFAOYSA-N 0.000 description 4
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 125000002947 alkylene group Chemical group 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 150000001721 carbon Chemical group 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 230000009477 glass transition Effects 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- OARRHUQTFTUEOS-UHFFFAOYSA-N safranin Chemical compound [Cl-].C=12C=C(N)C(C)=CC2=NC2=CC(C)=C(N)C=C2[N+]=1C1=CC=CC=C1 OARRHUQTFTUEOS-UHFFFAOYSA-N 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 150000005846 sugar alcohols Polymers 0.000 description 3
- BIAAQBNMRITRDV-UHFFFAOYSA-N 1-(chloromethoxy)-2-methoxyethane Chemical compound COCCOCCl BIAAQBNMRITRDV-UHFFFAOYSA-N 0.000 description 2
- RNIPJYFZGXJSDD-UHFFFAOYSA-N 2,4,5-triphenyl-1h-imidazole Chemical compound C1=CC=CC=C1C1=NC(C=2C=CC=CC=2)=C(C=2C=CC=CC=2)N1 RNIPJYFZGXJSDD-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- XLLIQLLCWZCATF-UHFFFAOYSA-N 2-methoxyethyl acetate Chemical compound COCCOC(C)=O XLLIQLLCWZCATF-UHFFFAOYSA-N 0.000 description 2
- 125000005916 2-methylpentyl group Chemical group 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N Bisphenol A Natural products C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 2
- 230000003190 augmentative effect Effects 0.000 description 2
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 2
- 239000012965 benzophenone Substances 0.000 description 2
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229920001400 block copolymer Polymers 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000007810 chemical reaction solvent Substances 0.000 description 2
- 230000001427 coherent effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000002542 deteriorative effect Effects 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- SHZIWNPUGXLXDT-UHFFFAOYSA-N ethyl hexanoate Chemical compound CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 description 2
- JVICFMRAVNKDOE-UHFFFAOYSA-M ethyl violet Chemical compound [Cl-].C1=CC(N(CC)CC)=CC=C1C(C=1C=CC(=CC=1)N(CC)CC)=C1C=CC(=[N+](CC)CC)C=C1 JVICFMRAVNKDOE-UHFFFAOYSA-M 0.000 description 2
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropyl acetate Chemical compound CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000012263 liquid product Substances 0.000 description 2
- 230000001404 mediated effect Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000005056 polyisocyanate Substances 0.000 description 2
- 229920005596 polymer binder Polymers 0.000 description 2
- 239000002491 polymer binding agent Substances 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 229920005604 random copolymer Polymers 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 150000003512 tertiary amines Chemical class 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 2
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 description 1
- NAMAKTDZWYRRPM-UHFFFAOYSA-N (2,5-dinitrophenyl)methyl 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)OCC1=CC([N+]([O-])=O)=CC=C1[N+]([O-])=O NAMAKTDZWYRRPM-UHFFFAOYSA-N 0.000 description 1
- DLDWUFCUUXXYTB-UHFFFAOYSA-N (2-oxo-1,2-diphenylethyl) 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)OC(C=1C=CC=CC=1)C(=O)C1=CC=CC=C1 DLDWUFCUUXXYTB-UHFFFAOYSA-N 0.000 description 1
- PVPBBTJXIKFICP-UHFFFAOYSA-N (7-aminophenothiazin-3-ylidene)azanium;chloride Chemical compound [Cl-].C1=CC(=[NH2+])C=C2SC3=CC(N)=CC=C3N=C21 PVPBBTJXIKFICP-UHFFFAOYSA-N 0.000 description 1
- WMAVHUWINYPPKT-UHFFFAOYSA-M (e)-3-methyl-n-[(e)-(1-methyl-2-phenylindol-1-ium-3-ylidene)amino]-1,3-thiazol-2-imine;chloride Chemical compound [Cl-].C12=CC=CC=C2N(C)C(C=2C=CC=CC=2)=C1N=NC=1SC=C[N+]=1C WMAVHUWINYPPKT-UHFFFAOYSA-M 0.000 description 1
- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 description 1
- FUOSTELFLYZQCW-UHFFFAOYSA-N 1,2-oxazol-3-one Chemical compound OC=1C=CON=1 FUOSTELFLYZQCW-UHFFFAOYSA-N 0.000 description 1
- ZOMLUNRKXJYKPD-UHFFFAOYSA-N 1,3,3-trimethyl-2-[2-(2-methylindol-3-ylidene)ethylidene]indole;hydrochloride Chemical compound [Cl-].C1=CC=C2C(C)(C)C(/C=C/C=3C4=CC=CC=C4NC=3C)=[N+](C)C2=C1 ZOMLUNRKXJYKPD-UHFFFAOYSA-N 0.000 description 1
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical compound C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 description 1
- VNQXSTWCDUXYEZ-UHFFFAOYSA-N 1,7,7-trimethylbicyclo[2.2.1]heptane-2,3-dione Chemical compound C1CC2(C)C(=O)C(=O)C1C2(C)C VNQXSTWCDUXYEZ-UHFFFAOYSA-N 0.000 description 1
- PPNCOQHHSGMKGI-UHFFFAOYSA-N 1-cyclononyldiazonane Chemical compound C1CCCCCCCC1N1NCCCCCCC1 PPNCOQHHSGMKGI-UHFFFAOYSA-N 0.000 description 1
- VZAWCLCJGSBATP-UHFFFAOYSA-N 1-cycloundecyl-1,2-diazacycloundecane Chemical compound C1CCCCCCCCCC1N1NCCCCCCCCC1 VZAWCLCJGSBATP-UHFFFAOYSA-N 0.000 description 1
- 125000006218 1-ethylbutyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C([H])([H])[H] 0.000 description 1
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 1
- VOGSDFLJZPNWHY-UHFFFAOYSA-N 2,2-difluoroethanol Chemical compound OCC(F)F VOGSDFLJZPNWHY-UHFFFAOYSA-N 0.000 description 1
- BYCNMZYQCQZYLG-UHFFFAOYSA-N 2,2-dimethoxy-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1.C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 BYCNMZYQCQZYLG-UHFFFAOYSA-N 0.000 description 1
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 description 1
- AZUHIVLOSAPWDM-UHFFFAOYSA-N 2-(1h-imidazol-2-yl)-1h-imidazole Chemical class C1=CNC(C=2NC=CN=2)=N1 AZUHIVLOSAPWDM-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- PTTPXKJBFFKCEK-UHFFFAOYSA-N 2-Methyl-4-heptanone Chemical compound CC(C)CC(=O)CC(C)C PTTPXKJBFFKCEK-UHFFFAOYSA-N 0.000 description 1
- BFMDZOWJRVLYPB-UHFFFAOYSA-N 2-[2-[2-(1,1-difluoro-2-hydroxyethoxy)-1,1,2,2-tetrafluoroethoxy]-1,1,2,2-tetrafluoroethoxy]-2,2-difluoroethanol Chemical compound OCC(F)(F)OC(F)(F)C(F)(F)OC(F)(F)C(F)(F)OC(F)(F)CO BFMDZOWJRVLYPB-UHFFFAOYSA-N 0.000 description 1
- UHFFVFAKEGKNAQ-UHFFFAOYSA-N 2-benzyl-2-(dimethylamino)-1-(4-morpholin-4-ylphenyl)butan-1-one Chemical compound C=1C=C(N2CCOCC2)C=CC=1C(=O)C(CC)(N(C)C)CC1=CC=CC=C1 UHFFVFAKEGKNAQ-UHFFFAOYSA-N 0.000 description 1
- 125000006176 2-ethylbutyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(C([H])([H])*)C([H])([H])C([H])([H])[H] 0.000 description 1
- SYMYWDHCQHTNJC-UHFFFAOYSA-J 3-oxobutanoate;zirconium(4+) Chemical compound [Zr+4].CC(=O)CC([O-])=O.CC(=O)CC([O-])=O.CC(=O)CC([O-])=O.CC(=O)CC([O-])=O SYMYWDHCQHTNJC-UHFFFAOYSA-J 0.000 description 1
- JJZNCUHIYJBAMS-UHFFFAOYSA-N 3-phenyl-2h-1,2-oxazol-5-one Chemical compound N1OC(=O)C=C1C1=CC=CC=C1 JJZNCUHIYJBAMS-UHFFFAOYSA-N 0.000 description 1
- KBQVDAIIQCXKPI-UHFFFAOYSA-N 3-trimethoxysilylpropyl prop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C=C KBQVDAIIQCXKPI-UHFFFAOYSA-N 0.000 description 1
- NDWUBGAGUCISDV-UHFFFAOYSA-N 4-hydroxybutyl prop-2-enoate Chemical compound OCCCCOC(=O)C=C NDWUBGAGUCISDV-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 150000007934 α,β-unsaturated carboxylic acids Chemical class 0.000 description 1
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Abstract
Description
−(R8O)n−R8−
[製造例1:シラン系官能基が分枝鎖に位置した(メタ)アクリレート系(共)重合体の製造方法]
2Lジャケット反応器にブチルアクリレート154g、KBM−503(3−メタクリロキシプロピルトリメトキシシラン) 46gを入れ、酢酸エチル800gで希釈した。約60〜70℃で反応温度をセッティングし、30分〜1時間程度攪拌を行った。n−ドデシルメルカプタン0.02gを追加で入れ、30分程度さらに攪拌を行った。その後、重合開始剤であるAIBN 0.06gを入れ、反応温度で4時間以上重合を行って残留アクリレート含有量が1%未満になるまで維持し、シラン系官能基が分枝鎖に位置した(メタ)アクリレート系(共)重合体(重量平均分子量約500,000〜600,000,Si−(OR)3当量1019g/当量)を製造した。
2Lジャケット反応器にブチルアクリレート180g、KBM−503(3−メタクリロキシプロピルトリメトキシシラン) 120gを入れ、酢酸エチル700gで希釈した。60〜70℃で反応温度をセッティングし、30分〜1時間程度攪拌を行った。n−ドデシルメルカプタン0.03gを追加で入れ、30分程度さらに攪拌を行った。その後、重合開始剤であるAIBN 0.09gを入れ、反応温度で4時間以上重合を行って残留アクリレート含有量が1%未満になるまで維持し、シラン系官能基が分枝鎖に位置した(メタ)アクリレート系(共)重合体(重量平均分子量約500,000〜600,000,Si−(OR)3当量586g/当量)を製造した。
2Lジャケット反応器にブチルアクリレート255g、KBM−503(3−メタクリロキシプロピルトリメトキシシラン) 45gを入れ、酢酸エチル700gで希釈した。60〜70℃で反応温度をセッティングし、30分〜1時間程度攪拌を行った。n−ドデシルメルカプタン0.03gを追加で入れ、30分程度さらに攪拌を行った。その後、重合開始剤であるAIBN 0.09gを入れ、反応温度で4時間以上重合を行って残留アクリレート含有量が1%未満になるまで維持し、シラン系官能基が分枝鎖に位置した(メタ)アクリレート系(共)重合体(重量平均分子量約500,000〜600,000,Si−(OR)3当量1562g/当量)を製造した。
1000mlフラスコにKBE−9007(3−イソシアナトプロピルトリエトキシシラン) 19.79g,PEG−400 12.80gとDBTDL 0.57gを入れ、テトラヒドロフラン300gで希釈した。TLCで反応物がすべて消耗したのが確認されるまで常温で攪拌した後、減圧して反応溶媒をすべて除去した。
1000mlフラスコに2,2’−((オキシビス(1,1,2,2−テトラフルオロエタン−2,1−ジイル))ビス(オキシ))ビス(2,2−ジフルオロエタン−1−オール)(2,2’−((oxybis(1,1,2,2−tetrafluoroethane−2,1−diyl))bis(oxy))bis(2,2−difluoroethan−1−ol))20.51gを入れた後、テトラヒドロフラン500gに溶かして0℃で攪拌しながら水素化ナトリウム(sodium hydride)(鉱油中60%分散体)4.40gを数回にわたって注意深く添加した。0℃で20分攪拌した後、2−メトキシエトキシメチルクロリド(2−methoxyethoxymethyl chloride)12.50mlをゆっくり滴下(dropping)した。1H NMRで反応物がすべて消耗したのが確認されると、減圧して反応溶媒をすべて除去した。ジクロロメタン300gで3回抽出して有機層を集めた後硫酸マグネシウム(magnesium sulfate)でフィルタした後減圧してジクロロメタンをすべて除去して純度95%以上の液状生成物29gを98%の収率で収得した。
1.フォトポリマー組成物の製造
下記表1または表2に記載されたように、前記製造例1ないし3で得たシラン重合体、光反応性単量体(高屈折アクリレート、屈折率1.600,HR6022[MIWON])、製造例5の非反応性低屈折物質、トリブチルホスフェート(Tributyl phosphate[TBP],分子量266.31,屈折率1.424,シグマアルドリッチ社製品)、safranin O(染料、シグマアルドリッチ社製品)、Ebecryl P−115(SK entis)、Borate V(Spectra group)、Irgacure 250(BASF)、シリコーン系反応性添加剤(Tego Rad 2500)およびメチルイソブチルケトン(MIBK)を光を遮断した状態で混合し、ペースト(Paste)ミキサーで約10分間攪拌して透明なコート液を収得した。
(1)前記製造されたフォトポリマーコーティング面をスライドガラスにラミネートし、記録時レーザがガラス面を先に通過するように固定した。
二つの干渉光(参照光および物体光)の干渉によりホログラフィックを記録し、透過型記録は二つのビームをサンプルの同一面に入射した。二つのビームの入射角により回折効率は変わるようになり、二つのビームの入射角が同じである場合non−slantedとなる。non−slanted記録は二ビームの入射角が法線基準に同一であるので、回折格子はフィルムに垂直に生成される。
透過型ホログラムの無損失誘電体格子(Lossless Dielectric grating)は、下記一般式2から屈折率変調値(△n)を計算することができる。
下記一般式3からレーザ損失量(Iloss)を計算することができる。
Iloss=1−{(PD+PT)/IO}
前記実施例で得られたホログラム媒体の一面に形成された線状パターンの形状および大きさをPark systems社の原子間力顕微鏡(XE7)を利用して測定した。そして、確認した表面形状からラインプロファイルを介して隣接する極小値と極大値との間の距離を測定した。
前記実施例で得られたホログラム媒体で基材と接する一面の表面エネルギを下記のような方法で測定した。
(1)ポリオールの合成
2Lのジャケット反応器にメチルアクリレート34.5g、ブチルアクリレート57.5g、4−ヒドロキシブチルアクリレート8gを入れ、酢酸エチル150gで希釈した。前記ジャケット反応器の温度を60〜70℃に維持しながら約1時間ほど攪拌を行った。そして、前記反応器にn−ドデシルメルカプタン0.035gを追加で入れ、30分程度さらに攪拌を行った。その後、重合開始剤AIBN(2,2’−アゾ−ビスイソブチロニトリル、2,2’−azo−bisisobutyronitrile) 0.04gを添加し、約70℃内外の温度で約4時間ほど重合し、残留するアクリレート類単量体の含有量1重量%になるまで維持し、ポリオールを合成した。この時、得られたポリオールはGPC法によって測定したポリスチレン換算の重量平均分子量が約70万であり、KOH滴定法を利用して測定したOH当量が1802g/OHmolであった。
前記製造例1のポリオール、光反応性単量体(高屈折アクリレート、屈折率1.600,HR6022[MIWON])、safranin O(染料、シグマアルドリッチ社製品)、製造例5の非反応性低屈折物質、トリブチルホスフェート(Tributyl phosphate[TBP],分子量266.31,屈折率1.424,シグマアルドリッチ社製品)、Ebecryl P−115 (SK entis)、Borate V (Spectra group)、Irgacure 250(BASF)およびメチルイソブチルケトン(MIBK)を光を遮断した状態で混合し、ペースト(Paste)ミキサーで約10分間攪拌して透明なコート液を収得した。
前記実施例と同様の方法でホログラム媒体を製造し、実施例と同様の方法および同じ条件で回折効率(η)、屈折率変調値(n)およびレーザ損失量(Iloss)を測定した。
前記実施例と同様の方法で比較例で得られたホログラム媒体の一面に形成された線状パターンの形状および大きさとホログラム媒体の表面を測定および観察した。
Claims (14)
- トリアセチルセルロース、脂環式オレフィン高分子およびポリエチレンテレフタレートからなる群より選ばれた1種以上の高分子を含む高分子樹脂層に比べてより高い表面エネルギを有する一面を有する、ホログラム記録媒体。
- ある一面の表面エネルギが50mN/m以上である、ホログラム記録媒体。
- 前記ホログラム記録媒体の一面は、50mN/m〜60mN/mの表面エネルギを有する、請求項1または2に記載のホログラム記録媒体。
- 前記ホログラム記録媒体は、シラン系官能基が主鎖または分枝鎖に位置する高分子樹脂を含む高分子基材を含む、請求項1から3のいずれか一項に記載のホログラム記録媒体。
- 前記高分子基材の他の一面には微細パターンが形成される、請求項4に記載のホログラム媒体。
- 前記微細パターンは、前記高分子基材の断面を基準に高さの極大値と高さの極小値が交互に繰り返される2以上の微細突起を含む形状を有し、
前記一つの微細突起の高さの極大値とこれと隣り合う微細突起の高さの極小値との間の前記高分子基材の断面方向に対する距離の標準誤差が20nm以下である、請求項5に記載のホログラム媒体。 - 前記一つの微細突起の高さの極大値とこれと隣り合う微細突起の高さの極小値との間の前記高分子基材の断面方向に対する距離は、0.2μm〜2μmである、請求項6に記載のホログラム媒体。
- 前記一つの微細突起の高さの極大値とこれと隣り合う微細突起の高さの極小値との間の差である振幅(Amplitude)が5〜50nmである、請求項6または7に記載のホログラム媒体。
- 前記高分子基材は、シラン系官能基が分枝鎖に位置する(メタ)アクリレート系(共)重合体およびシラン架橋剤を含む高分子マトリックスと;光反応性単量体と;の間の架橋結合物を含む、請求項4から8のいずれか一項に記載のホログラム媒体。
- 前記高分子マトリックスは、前記シラン系官能基が分枝鎖に位置する(メタ)アクリレート系(共)重合体100重量部に対して前記シラン架橋剤10重量部〜90重量部を含む、請求項9に記載のホログラム媒体。
- 前記シラン系官能基が分枝鎖に位置する(メタ)アクリレート系(共)重合体は、300g/当量〜2000g/当量のシラン系官能基の当量を有する、請求項9または10に記載のホログラム媒体。
- 前記シラン架橋剤は、重量平均分子量が100〜2000である線状のポリエーテル主鎖および前記主鎖の末端または分枝鎖で結合したシラン系官能基を含む、請求項9から11のいずれか一項に記載のホログラム媒体。
- 前記高分子基材は、エーテル基、エステル基およびアミド基からなる群より選ばれた1種以上の官能基および2以上のジフルオロメチレン基を含むフッ素系化合物をさらに含む、請求項4から12のいずれか一項に記載のホログラム媒体。
- 請求項1から13のいずれか一項に記載のホログラム媒体を含む、光学素子。
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