CN115710438B - Metal oxide dispersion, thin film composition for display, and optical element for display - Google Patents
Metal oxide dispersion, thin film composition for display, and optical element for display Download PDFInfo
- Publication number
- CN115710438B CN115710438B CN202211005154.0A CN202211005154A CN115710438B CN 115710438 B CN115710438 B CN 115710438B CN 202211005154 A CN202211005154 A CN 202211005154A CN 115710438 B CN115710438 B CN 115710438B
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- China
- Prior art keywords
- acrylate
- metal oxide
- methacrylate
- group
- oxide dispersion
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- 239000006185 dispersion Substances 0.000 title claims abstract description 95
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 74
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 74
- 239000000203 mixture Substances 0.000 title claims abstract description 29
- 230000003287 optical effect Effects 0.000 title claims abstract description 17
- 239000010409 thin film Substances 0.000 title claims description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 110
- 239000000178 monomer Substances 0.000 claims abstract description 43
- 239000002105 nanoparticle Substances 0.000 claims abstract description 33
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000003607 modifier Substances 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims description 51
- -1 diphenyl acrylate Chemical compound 0.000 claims description 48
- 239000010408 film Substances 0.000 claims description 22
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 18
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 12
- 229920000570 polyether Polymers 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 9
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 8
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000012788 optical film Substances 0.000 claims description 8
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 8
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 7
- 239000012952 cationic photoinitiator Substances 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 229910000077 silane Inorganic materials 0.000 claims description 7
- QUEWJUQWKGAHON-UHFFFAOYSA-N (2-phenylphenyl) 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=CC=C1C1=CC=CC=C1 QUEWJUQWKGAHON-UHFFFAOYSA-N 0.000 claims description 6
- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical compound C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 claims description 6
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 claims description 6
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- 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 claims description 6
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 6
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 125000003545 alkoxy group Chemical group 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 6
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 6
- MUTNCGKQJGXKEM-UHFFFAOYSA-N tamibarotene Chemical compound C=1C=C2C(C)(C)CCC(C)(C)C2=CC=1NC(=O)C1=CC=C(C(O)=O)C=C1 MUTNCGKQJGXKEM-UHFFFAOYSA-N 0.000 claims description 6
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical compound CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 claims description 5
- ZDQNWDNMNKSMHI-UHFFFAOYSA-N 1-[2-(2-prop-2-enoyloxypropoxy)propoxy]propan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COCC(C)OC(=O)C=C ZDQNWDNMNKSMHI-UHFFFAOYSA-N 0.000 claims description 5
- CYKONRWVCOIAHL-UHFFFAOYSA-N 5-(oxiran-2-yl)pentyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCC1CO1 CYKONRWVCOIAHL-UHFFFAOYSA-N 0.000 claims description 5
- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- 125000003277 amino group Chemical group 0.000 claims description 5
- 235000010290 biphenyl Nutrition 0.000 claims description 5
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical group Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 5
- 125000003700 epoxy group Chemical group 0.000 claims description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 5
- ZMZHRHTZJDBLEX-UHFFFAOYSA-N (2-phenylphenyl) prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1C1=CC=CC=C1 ZMZHRHTZJDBLEX-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- GSJNBCZKEUYYLK-UHFFFAOYSA-N [phenoxy(phenyl)methyl] prop-2-enoate Chemical compound C=1C=CC=CC=1C(OC(=O)C=C)OC1=CC=CC=C1 GSJNBCZKEUYYLK-UHFFFAOYSA-N 0.000 claims description 4
- AOJOEFVRHOZDFN-UHFFFAOYSA-N benzyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC1=CC=CC=C1 AOJOEFVRHOZDFN-UHFFFAOYSA-N 0.000 claims description 4
- 239000004305 biphenyl Substances 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- QIWKUEJZZCOPFV-UHFFFAOYSA-N phenyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=CC=C1 QIWKUEJZZCOPFV-UHFFFAOYSA-N 0.000 claims description 4
- WRAQQYDMVSCOTE-UHFFFAOYSA-N phenyl prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1 WRAQQYDMVSCOTE-UHFFFAOYSA-N 0.000 claims description 4
- 150000003254 radicals Chemical class 0.000 claims description 4
- YKZMWXJHPKWFLS-UHFFFAOYSA-N (2-chlorophenyl) 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=CC=C1Cl YKZMWXJHPKWFLS-UHFFFAOYSA-N 0.000 claims description 3
- GOUZWCLULXUQSR-UHFFFAOYSA-N (2-chlorophenyl) prop-2-enoate Chemical compound ClC1=CC=CC=C1OC(=O)C=C GOUZWCLULXUQSR-UHFFFAOYSA-N 0.000 claims description 3
- WBBKYDCLZKGNSD-UHFFFAOYSA-N (2-nitrophenyl)methyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC1=CC=CC=C1[N+]([O-])=O WBBKYDCLZKGNSD-UHFFFAOYSA-N 0.000 claims description 3
- BRXDAEMGSYZHGK-UHFFFAOYSA-N (4-bromophenyl)-trimethoxysilane Chemical compound CO[Si](OC)(OC)C1=CC=C(Br)C=C1 BRXDAEMGSYZHGK-UHFFFAOYSA-N 0.000 claims description 3
- XSQUPVXOENTCJV-UHFFFAOYSA-N (6-phenylpyridin-3-yl)boronic acid Chemical compound N1=CC(B(O)O)=CC=C1C1=CC=CC=C1 XSQUPVXOENTCJV-UHFFFAOYSA-N 0.000 claims description 3
- UIQCRIFSBWGDTQ-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,10,10,10-heptadecafluorodecyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F UIQCRIFSBWGDTQ-UHFFFAOYSA-N 0.000 claims description 3
- CEXMTZSYTLNAOG-UHFFFAOYSA-N 1,1,2,3,3,3-hexafluoropropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(F)(F)C(F)C(F)(F)F CEXMTZSYTLNAOG-UHFFFAOYSA-N 0.000 claims description 3
- HFGOJHZGZKOYOH-UHFFFAOYSA-N 1-(2-methoxyphenyl)-4-[(2-phenylphenyl)methyl]piperazine Chemical compound COC1=CC=CC=C1N1CCN(CC=2C(=CC=CC=2)C=2C=CC=CC=2)CC1 HFGOJHZGZKOYOH-UHFFFAOYSA-N 0.000 claims description 3
- WZFAVDDTRQICHQ-UHFFFAOYSA-N 1-(3-methoxyphenyl)-4-[(2-phenylphenyl)methyl]piperazine Chemical compound COC1=CC=CC(N2CCN(CC=3C(=CC=CC=3)C=3C=CC=CC=3)CC2)=C1 WZFAVDDTRQICHQ-UHFFFAOYSA-N 0.000 claims description 3
- OCJKEFFQAUMPTO-UHFFFAOYSA-N 1-(4-methoxyphenyl)-4-[(2-phenylphenyl)methyl]piperazine Chemical compound C1=CC(OC)=CC=C1N1CCN(CC=2C(=CC=CC=2)C=2C=CC=CC=2)CC1 OCJKEFFQAUMPTO-UHFFFAOYSA-N 0.000 claims description 3
- SQQZOCBNDHOJEJ-UHFFFAOYSA-N 1-[(2-phenylphenyl)methyl]-4-(2-propan-2-yloxyphenyl)piperazine Chemical compound CC(C)OC1=CC=CC=C1N1CCN(CC=2C(=CC=CC=2)C=2C=CC=CC=2)CC1 SQQZOCBNDHOJEJ-UHFFFAOYSA-N 0.000 claims description 3
- UCRKMUUOHCZVJX-UHFFFAOYSA-N 1-phenyl-4-[(2-phenylphenyl)methyl]piperazine Chemical compound C=1C=CC=C(C=2C=CC=CC=2)C=1CN(CC1)CCN1C1=CC=CC=C1 UCRKMUUOHCZVJX-UHFFFAOYSA-N 0.000 claims description 3
- KBRVQAUYZUFKAJ-UHFFFAOYSA-N 1-trimethoxysilylpropan-2-amine Chemical compound CO[Si](OC)(OC)CC(C)N KBRVQAUYZUFKAJ-UHFFFAOYSA-N 0.000 claims description 3
- VBHXIMACZBQHPX-UHFFFAOYSA-N 2,2,2-trifluoroethyl prop-2-enoate Chemical compound FC(F)(F)COC(=O)C=C VBHXIMACZBQHPX-UHFFFAOYSA-N 0.000 claims description 3
- FTALTLPZDVFJSS-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl prop-2-enoate Chemical compound CCOCCOCCOC(=O)C=C FTALTLPZDVFJSS-UHFFFAOYSA-N 0.000 claims description 3
- CBKJLMZJKHOGEQ-UHFFFAOYSA-N 2-(oxiran-2-yl)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCC1CO1 CBKJLMZJKHOGEQ-UHFFFAOYSA-N 0.000 claims description 3
- WDQMWEYDKDCEHT-UHFFFAOYSA-N 2-ethylhexyl 2-methylprop-2-enoate Chemical compound CCCCC(CC)COC(=O)C(C)=C WDQMWEYDKDCEHT-UHFFFAOYSA-N 0.000 claims description 3
- RZVINYQDSSQUKO-UHFFFAOYSA-N 2-phenoxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC1=CC=CC=C1 RZVINYQDSSQUKO-UHFFFAOYSA-N 0.000 claims description 3
- GXDMUOPCQNLBCZ-UHFFFAOYSA-N 3-(3-triethoxysilylpropyl)oxolane-2,5-dione Chemical compound CCO[Si](OCC)(OCC)CCCC1CC(=O)OC1=O GXDMUOPCQNLBCZ-UHFFFAOYSA-N 0.000 claims description 3
- PMJIKKNFJBDSHO-UHFFFAOYSA-N 3-[3-aminopropyl(diethoxy)silyl]oxy-3-methylpentane-1,5-diol Chemical compound NCCC[Si](OCC)(OCC)OC(C)(CCO)CCO PMJIKKNFJBDSHO-UHFFFAOYSA-N 0.000 claims description 3
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 claims description 3
- FMGBDYLOANULLW-UHFFFAOYSA-N 3-isocyanatopropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCN=C=O FMGBDYLOANULLW-UHFFFAOYSA-N 0.000 claims description 3
- YATIYDNBFHEOFA-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-ol Chemical compound CO[Si](OC)(OC)CCCO YATIYDNBFHEOFA-UHFFFAOYSA-N 0.000 claims description 3
- KBQVDAIIQCXKPI-UHFFFAOYSA-N 3-trimethoxysilylpropyl prop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C=C KBQVDAIIQCXKPI-UHFFFAOYSA-N 0.000 claims description 3
- LVACOMKKELLCHJ-UHFFFAOYSA-N 3-trimethoxysilylpropylurea Chemical compound CO[Si](OC)(OC)CCCNC(N)=O LVACOMKKELLCHJ-UHFFFAOYSA-N 0.000 claims description 3
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 3
- SAPGBCWOQLHKKZ-UHFFFAOYSA-N 6-(2-methylprop-2-enoyloxy)hexyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCCCCOC(=O)C(C)=C SAPGBCWOQLHKKZ-UHFFFAOYSA-N 0.000 claims description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical class CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 235000000126 Styrax benzoin Nutrition 0.000 claims description 3
- 244000028419 Styrax benzoin Species 0.000 claims description 3
- 235000008411 Sumatra benzointree Nutrition 0.000 claims description 3
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical class NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 150000004056 anthraquinones Chemical class 0.000 claims description 3
- 239000012965 benzophenone Substances 0.000 claims description 3
- 150000008366 benzophenones Chemical class 0.000 claims description 3
- OIWOHHBRDFKZNC-UHFFFAOYSA-N cyclohexyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1CCCCC1 OIWOHHBRDFKZNC-UHFFFAOYSA-N 0.000 claims description 3
- 239000012954 diazonium Substances 0.000 claims description 3
- 150000001989 diazonium salts Chemical class 0.000 claims description 3
- WHGNXNCOTZPEEK-UHFFFAOYSA-N dimethoxy-methyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](C)(OC)CCCOCC1CO1 WHGNXNCOTZPEEK-UHFFFAOYSA-N 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 3
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 3
- 239000012949 free radical photoinitiator Substances 0.000 claims description 3
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 3
- 235000019382 gum benzoic Nutrition 0.000 claims description 3
- 150000002460 imidazoles Chemical class 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 3
- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 claims description 3
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims description 3
- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 claims description 3
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 claims description 3
- 150000002923 oximes Chemical class 0.000 claims description 3
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 claims description 3
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 claims description 3
- FSDNTQSJGHSJBG-UHFFFAOYSA-N piperidine-4-carbonitrile Chemical compound N#CC1CCNCC1 FSDNTQSJGHSJBG-UHFFFAOYSA-N 0.000 claims description 3
- QCTJRYGLPAFRMS-UHFFFAOYSA-N prop-2-enoic acid;1,3,5-triazine-2,4,6-triamine Chemical compound OC(=O)C=C.NC1=NC(N)=NC(N)=N1 QCTJRYGLPAFRMS-UHFFFAOYSA-N 0.000 claims description 3
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 3
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- AFFZTFNQQHNSEG-UHFFFAOYSA-N trifluoromethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(F)(F)F AFFZTFNQQHNSEG-UHFFFAOYSA-N 0.000 claims description 3
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 claims description 3
- SEKZHGKCVMOJSY-UHFFFAOYSA-N [dimethoxy(propyl)silyl]oxymethyl 2-methylprop-2-enoate Chemical compound CCC[Si](OC)(OC)OCOC(=O)C(C)=C SEKZHGKCVMOJSY-UHFFFAOYSA-N 0.000 claims description 2
- DRRZZMBHJXLZRS-UHFFFAOYSA-N n-[3-[dimethoxy(methyl)silyl]propyl]cyclohexanamine Chemical compound CO[Si](C)(OC)CCCNC1CCCCC1 DRRZZMBHJXLZRS-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 2
- KBFMLDFKMYHWRP-UHFFFAOYSA-N 1-(2-ethoxyphenyl)-4-[(2-phenylphenyl)methyl]piperazine Chemical compound CCOC1=CC=CC=C1N1CCN(CC=2C(=CC=CC=2)C=2C=CC=CC=2)CC1 KBFMLDFKMYHWRP-UHFFFAOYSA-N 0.000 claims 1
- CEXQWAAGPPNOQF-UHFFFAOYSA-N 2-phenoxyethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOC1=CC=CC=C1 CEXQWAAGPPNOQF-UHFFFAOYSA-N 0.000 claims 1
- 229930185605 Bisphenol Natural products 0.000 claims 1
- LCXXNKZQVOXMEH-UHFFFAOYSA-N Tetrahydrofurfuryl methacrylate Chemical compound CC(=C)C(=O)OCC1CCCO1 LCXXNKZQVOXMEH-UHFFFAOYSA-N 0.000 claims 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract description 5
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract description 5
- 239000002245 particle Substances 0.000 description 27
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- 238000000034 method Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 10
- 238000009792 diffusion process Methods 0.000 description 6
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
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Classifications
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
- C08F2/50—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light with sensitising agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F20/02—Monocarboxylic acids having less than ten carbon atoms, Derivatives thereof
- C08F20/10—Esters
- C08F20/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F20/32—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F22/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides or nitriles thereof
- C08F22/10—Esters
- C08F22/12—Esters of phenols or saturated alcohols
- C08F22/20—Esters containing oxygen in addition to the carboxy oxygen
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
- C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
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- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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Abstract
The invention relates to a metal oxide dispersion, a film composition for a display and an optical element for a display, wherein the metal oxide dispersion comprises zirconium oxide nano particles according to one embodiment of the invention; a monomer; and a surface modifier, wherein the zirconia nanoparticle has a tetragonal full width at half maximum (FWHM) of 0.9 or more and a monoclinic full width at half maximum (FWHM) of 0.7 or more.
Description
Technical Field
The invention relates to a metal oxide dispersion, a thin film composition for a display, and an optical element for a display.
Background
Optically transparent polymer materials are widely used for optical coatings and optoelectronic materials because of their low cost, good processability and high visible light transmittance, but it is difficult to achieve a high refractive index only with polymer materials, so methods of mixing metal oxide particles having a high refractive index into polymers and dispersing them are actively being developed.
In order to realize the high brightness, high contrast, low power consumption, and other properties of the display, organic-inorganic hybrid materials having high refractive index metal oxide particles are used as transparent materials for the display, and are expected to be widely used in the future.
However, although the organic-inorganic hybrid material having high refractive index metal oxide particles can increase the refractive index by the metal oxide particles, optical properties such as light transmittance, haze (haze), yellowness (y.i.), and the like are simultaneously reduced, and are limited in use as a display material.
To solve this problem, many techniques have been studied on how to improve yellowness while maintaining physical properties such as refractive index, viscosity, etc., and these techniques have generally changed the synthesis method of inorganic substances or used additives in large amounts, and have a problem of affecting other physical properties.
Accordingly, there is a need for a technique for preparing a metal oxide particle dispersion that can improve the yellowness of an organic-inorganic hybrid material having high refractive metal oxide particles without affecting other physical properties.
The foregoing background is what the inventors have learned or learned during the development of the invention and should not be construed as essential to the general knowledge of the technology disclosed before the application of the invention.
Disclosure of Invention
Problems to be solved by the invention
The present invention has been made to solve the above-mentioned problems, and provides a metal oxide dispersion, a thin film composition for display, and an optical element for display, which can achieve a high refractive index and low yellowness by adjusting a mixing ratio of crystal phases of zirconia nanoparticles.
The technical problems to be solved by the present invention are not limited to the above-described problems, and other problems not described will be clearly understood by those skilled in the art from the following description.
Technical means for solving the problems
A metal oxide dispersion according to an embodiment of the present invention may include: zirconia nanoparticles; a monomer; and a surface modifier, wherein the zirconia nanoparticle has a tetragonal full width at half maximum (full width at half maximum, FWHM) of 0.9 or more and a monoclinic full width at half maximum of 0.7 or more.
According to an embodiment, the zirconia nanoparticles may have a crystal size of less than 10nm.
According to an embodiment, the volume fraction (Vm) of the monoclinic system calculated by the following equations 1 and 2 may be 30% to 40%,
the tetragonal system volume fraction (Vt) calculated by the following equation 3 may be 60% to 70%:
[ formula 1]
[ formula 2]
And
V m : volume fraction of monoclinic system
(111): for->(111) Monoclinic system strength of peak of plane
It (101): tetragonal strength of peak for (101) plane
[ formula 3]
Vt＝1-Vm
V t : volume fraction of tetragonal system.
According to an embodiment, the zirconia nanoparticles may be 40 wt% to 70 wt% of the metal oxide dispersion.
In accordance with one embodiment of the present invention, the monomers may be selected from the group consisting of methyl acrylate, lauryl acrylate, ethoxydiglycol acrylate, methoxytriglycol acrylate, phenoxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxy-3-phenoxyacrylate, neopentyl glycol diacrylate, 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate, trimethylolpropane acrylate, trimethylolpropane benzoate, methyl methacrylate, 2-ethylhexyl methacrylate, octadecyl methacrylate, cyclohexyl methacrylate, tetrahydrofurfuryl methacrylate phenoxyethyl methacrylate, methoxypolyethylene methacrylate, 2-hydroxyethyl methacrylate, 2-hydroxybutyl methacrylate, heptadecafluorodecyl methacrylate, trifluoromethyl methacrylate, trifluoroethyl acrylate, hexafluoropropyl methacrylate, 1, 6-hexanediol dimethacrylate, trimethylolpropane trimethacrylate, glycerol dimethacrylate hexamethylene diisocyanate, ethylene glycol dimethacrylate, urethane acrylate, epoxy acrylate, melamine acrylate, benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, 2- ([ 1,1' -biphenyl ] -2-oxy) ethyl acrylate, phenoxybenzyl acrylate, 3-phenoxybenzyl-3- (1-naphthyl) acrylate, ethyl (2E) -3-hydroxy-2- (3-phenoxybenzyl) acrylate, phenyl methacrylate, biphenyl methacrylate, 2-nitrophenyl acrylate, 4-nitrophenyl acrylate, 2-nitrophenyl methacrylate, 4-nitrophenyl methacrylate, 2-nitrobenzyl methacrylate, 4-nitrobenzyl methacrylate, 2-chlorophenyl acrylate, 4-chlorophenyl acrylate, 2-chlorophenyl methacrylate, 4-chlorophenyl methacrylate, ethyl o-phenylphenol acrylate, phenol, biphenyl methacrylate, o-phenylphenol ethoxyacrylate, 1- (biphenyl-2-ylmethyl) -4-phenylpiperazine, 1- (biphenyl-2-ylmethyl) -4- (2-methoxyphenyl) piperazine, 1- (biphenyl-2-ethoxyphenyl) -4- (2-ethoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (2-isopropoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (3-methoxyphenyl) piperazine, at least one selected from the group consisting of 1- (biphenyl-2-ylmethyl) -4- (4-methoxyphenyl) piperazine and bisphenol-diacrylate.
According to an embodiment, the monomer may be 1 to 50 wt% of the metal oxide dispersion.
According to an embodiment, the surface modifier may include a silane coupling agent, which may be a silane including at least one selected from the group consisting of an acrylate group, (meth) acrylic group, epoxy group (epoxy group), alkoxy group (alkoxy), vinyl group (vinyl group), phenyl group (phenyl group), methacryloxy group (metacryloxy group), amino group (amino group), chlorosilane group (chlorosilane group), chloropropyl group (chloropropyl) and mercapto group (mercapto).
According to one embodiment, the surface modifier may include a surfactant selected from the group consisting of gamma-methacryloxypropyl trimethoxysilane, 4-aminobutyl methyl diethoxysilane, 3-aminopropyl trimethoxysilane, N-2-aminoethyl-3-aminopropyl diethyl isopropoxysilane, (mercaptomethyl) dimethylethoxysilane, di-4-mercaptobutyl dimethoxysilane, 3-mercaptopropyl triisopropoxysilane, 3-methacryloxypropyl dimethylethoxysilane, 3-acryloxypropyl trimethoxysilane, (3-glycidoxypropyl) methyldimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, 3-chloropropyltrimethoxysilane, 4-bromobutyl methyldibutoxysilane, 5-iodohexyl diethyl methoxysilane, 3-isocyanatopropyl trimethoxysilane, 3-isothiocyanate propylmethyldimethoxysilane, 3-hydroxybutyl isopropyl dimethoxysilane, bis (2-hydroxyethyl) -3-aminopropyl triethoxysilane, bromophenyl trimethoxysilane, (2- (iodophenyl) ethyl) dimethoxysilane, bis (chlorophenyl) ethyltrimethoxysilane, bis- (dimethoxyphenyl) dimethoxysilane, N-dimethoxypropyl-N-propyliminopropyl-dimethoxysilane, N-dimethoxypropyl-N- (propyliminomethyl) propyldimethoxysilane, N-propyliminomethyl-ethyl-3-propyltrimethoxysilane, N-propyliminomethyl-propyl-methyl-propyl-2-ethoxysilane, and N-propylethoxymethyl-propyl-ethoxysilane At least one selected from the group consisting of 3- (trimethoxysilyl) propanol, (3, 5-hexanedione) triethoxysilane, 3- (trimethoxysilyl) propylacetoacetate, 3- (trimethoxysilyl) propylmethacrylate silane, 3-aminopropyl trimethoxysilane, 2-aminopropyl trimethoxysilane, N- (2-aminoethyl) -3-aminopropyl methyldimethoxysilane, 3-ureidopropyl trimethoxysilane, N-ethoxycarbonyl-3-aminopropyl trimethoxysilane, N-triethoxysilylpropyl triethyltriamine, N-trimethoxysilylpropyl triethyltriamine, 10-trimethoxysilyl-1, 4, 7-triazoldecane, 10-triethoxysilyl-1, 4, 7-triazoldecane, 9-trimethoxysilyl-3, 6-azo-nonaneacetate, 3- (triethoxysilyl) propylsuccinic anhydride, N-benzyl-3-aminopropyl trimethoxysilane, N-phenyl-3-aminopropyl trimethoxysilane, N-dioxyvinyl-3-aminopropyl trimethoxysilane and (methacryloxypropyl) trimethoxysilane.
According to an embodiment, the surface modifier may be 1 to 50 wt% of the metal oxide dispersion.
According to an embodiment, the metal oxide dispersion may further include a dispersant including at least one selected from the group consisting of a polyether acid-based compound, a polyether amine-based compound, a polyether acid/amine mixture, an ester-based compound including a phosphoric acid group, and a polyether-based compound including a phosphoric acid group.
According to one embodiment, the metal oxide dispersion may be solvent-free.
According to an embodiment, the viscosity of the metal oxide dispersion may be 200cP to 50000cP.
According to an embodiment, the refractive index of the metal oxide dispersion may be 1.60 or more.
According to one embodiment, the metal oxide dispersion may have a yellowness (Yellow Index; Y.I) of 30 or less and a Haze (Haze) of 20 or less.
A film composition for a display according to another embodiment of the present invention includes: a metal oxide dispersion according to an embodiment of the present invention; a UV photoinitiator; and a UV curable monomer.
According to an embodiment, the UV photoinitiator may include at least any one selected from the group consisting of a cationic photoinitiator and a radical photoinitiator, wherein the cationic photoinitiator is selected from the group consisting of onium salts, diazonium salts, sulfonium salt compounds, and imidazoles; the free radical photoinitiator is selected from thioxanthones, phosphites, triazines, benzophenones, benzoins, oximes, acetones, aminoketones, ketones, benzoin ether acetophenones, anthraquinones and aromatic phosphine oxides.
According to an embodiment, the UV curable monomer may include at least one selected from the group consisting of glycidyl acrylate, glycidyl methacrylate, glycidyl- α -ethyl acrylate, glycidyl- α -n-propyl acrylate, glycidyl- α -butyl acrylate, 3, 4-epoxybutyl methacrylate, 3, 4-epoxybutyl acrylate, methyl 6, 7-epoxyheptyl methacrylate, 6, 7-epoxyheptyl acrylate, 6, 7-epoxyheptyl- α -ethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl methacrylate, tripropylene glycol diacrylate, dipropylene glycol diacrylate, 1, 6-hexanediol diacrylate, and trimethylolpropane triacrylate.
An optical film according to still another embodiment of the present invention includes a cured product of the dispersion composition for a display according to an embodiment of the present invention.
An optical element for a display according to still another embodiment of the present invention includes the diffusion film of an embodiment of the present invention.
ADVANTAGEOUS EFFECTS OF INVENTION
According to the metal oxide dispersion liquid, the volume fraction of the mixed crystal phase of the zirconia nano particles is adjusted to prepare the acrylate monomer mixed dispersion liquid with low yellowness and high refractive index. The zirconia nanoparticles having a crystal structure in which the mixing ratio is adjusted can be determined based on the mixing ratio as to the full width at half maximum of the crystal structure and the crystal size. The zirconia particles of the metal oxide dispersion have excellent dispersibility, and have excellent fluidity and moldability due to low viscosity, and thus can be used as an element, that is, as a sol dispersion for a display, which improves the efficiency of a display device.
The diffusion film according to an embodiment of the present invention and the optical element for display can be used to manufacture a diffusion film for a backlight unit of a mobile phone, a tablet computer, a PDP, a notebook computer, a display screen, a TV.
Drawings
Fig. 1 is a drawing illustrating the crystal structure and density of a general zirconia particle.
Fig. 2 is a drawing illustrating measurement of crystal size of crystal structure of zirconia nanoparticles according to an embodiment of the present invention.
Detailed Description
Hereinafter, embodiments will be described in detail with reference to the accompanying drawings. It should be understood that various changes may be made to the embodiments and that the scope of the application is not limited to the following examples. All changes made to the embodiments, and equivalents and alternatives thereof, are intended to be within the scope of the invention.
The terminology used in the implementations is for the purpose of describing particular embodiments only and is not intended to be limiting of scope. Where not specifically stated in the context, singular expressions include plural meanings. In this specification, the terms "comprises" and "comprising," and the like, are used to specify the presence of stated features, integers, steps, operations, elements, components, or groups thereof, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, or groups thereof.
All terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art without other definitions. Terms commonly used as dictionary defined should be understood as meaning in the related art, and should not be interpreted as idealized or excessively formalized meaning without being explicitly defined in the specification.
In the description with reference to the drawings, the same reference numerals are used for the same components irrespective of the reference numerals, and duplicate descriptions are omitted. In describing the embodiments, when it is judged that detailed description of the related art will unnecessarily obscure the embodiments, detailed description thereof will be omitted.
In describing the constituent elements of the embodiment, the terms of first, second, A, B, (a), (b) and the like may be used. These terms are only used to distinguish one component from another and are not used to limit the nature or order of the corresponding components, etc.
When one component has a common function with a component of one embodiment, the same name is used to describe the component in other embodiments. In the case where the contrary is not mentioned, the description of one embodiment can be applied to other embodiments, and the detailed description is omitted for repeated matters.
A metal oxide dispersion according to an embodiment of the present invention includes zirconia nanoparticles; a monomer; and a surface modifier, wherein the zirconia nanoparticle has a tetragonal full width at half maximum (full width at half maximum, FWHM) of 0.9 or more and a monoclinic full width at half maximum of 0.7 or more.
Fig. 1 is a drawing illustrating the crystal structure and density of a general zirconia particle.
Referring to fig. 1, the general zirconia particles have 3 crystal phases such as monoclinic (monoclinic), tetragonal (tetragonal), and cubic (cubic) according to the a, b, and c3 crystal axes forming the crystals.
The monoclinic crystal phase remains stable until 1400K, from 1170K to 2640K is tetragonal crystal phase, and from higher temperature to melting point is cubic crystal phase, and the theoretical density is shown in the figure.
The metal oxide dispersion liquid according to an embodiment of the present invention includes a structure in which tetragonal system and monoclinic system are mixed in a mixed crystal phase of nano zirconia.
The metal oxide dispersion according to an embodiment of the present invention can provide a dispersion with low yellowness (Y.I) and high refractive index by adjusting the volume fraction of tetragonal system (2θ= 30.119 °) and monoclinic system (2θ= 28.217 °) in the mixed crystal phase of nano zirconia.
Fig. 2 is a drawing illustrating measurement of crystal size of crystal structure of zirconia nanoparticles according to an embodiment of the present invention.
According to one embodiment, the zirconia nanoparticle crystal size (crystalline size) is the average of all zirconia nanoparticles in all metal oxide dispersions, as shown by the crystal size in fig. 2. A representative sample of the metal oxide dispersion may be collected and the crystal size of the zirconia nanoparticles measured using a Scanning Electron Microscope (SEM).
According to an embodiment, the zirconia nanoparticles may have a crystal size of less than 10nm. When the zirconia particles D 50 When the average crystal size exceeds 10nm, scattering or scattering occursAgglomeration or precipitation occurs, which can lead to unacceptable coating appearance and reduced refractive index.
According to an embodiment, the volume fraction (Vm) of the monoclinic system (2θ= 28.217 °) calculated by the following equations 1 and 2 may be 30% to 40%; the volume fraction (Vt) of the tetragonal system (2θ= 30.119 °) calculated by the following equation 3 may be 60% to 70%.
[ formula 1]
[ formula 2]
And
V m : volume fraction of monoclinic system
(111): for- >(111) Monoclinic system strength of peak of plane
It (101): tetragonal strength of peak for (101) plane
[ formula 3]
Vt＝1-Vm
V t : tetragonal system volume fraction
Preferably, the volume fraction (Vm) of the monoclinic system may be 34% to 40%, or 36% to 40%; the volume fraction (Vt) of the tetragonal system may be 60% to 65%, or 60% to 63%, and by adjusting the volume fraction of the mixed crystal phase of the zirconia particles, yellowness can be reduced while achieving a high refractive index.
According to an embodiment, the zirconia nanoparticles may be 40 wt% to 70 wt% of the metal oxide dispersion. Below 40 wt% of the metal oxide dispersion, the brightness of the curable composition is reduced, which reduces the optical properties of the cured film produced in the subsequent process; when the amount exceeds 70% by weight, the dispersion interval between the zirconia nanoparticles is rapidly reduced, and the viscosity of the dispersion is excessively increased, so that the zirconia nanoparticles are aggregated.
Preferably, the zirconia nanoparticles may be 50 wt% to 70 wt%, 60 wt% to 70 wt%, 40 wt% to 60 wt%, 50 wt% to 60 wt%, or 40 wt% to 50 wt% in the metal oxide dispersion.
According to an embodiment, the monomer may include at least one selected from the group consisting of C1 to C22 alkyl acrylate monomers, C1 to C22 alkoxy acrylate monomers, C6 to C24 aryl acrylate monomers, C1 to C22 alkyl (meth) acrylate monomers, C1 to C22 alkoxy (meth) acrylate monomers, C6 to C24 aryl (meth) acrylate monomers, alkylene glycol di (meth) acrylate monomers, alkylene glycol diacrylate monomers, alkylene glycol alkyl ether (meth) acrylate monomers, alkylene glycol alkyl ether acrylate monomers, derivatives incorporating methacrylate and/or acrylate substituents.
And, the molecule of the monomer is again substituted with at least one of a hydroxyl group, an aliphatic ring, and an aromatic ring (6 to 30 carbons), the "alkylene" has 1 to 10 carbons, including 1 to 20 (n), and the "alkyl ether" may include an alkyl group of 1 to 20 carbons. The monomers may include functional acrylates of 1 to 6, such as difunctional, trifunctional, and the like.
In accordance with one embodiment of the present invention, the monomers may be selected from the group consisting of methyl acrylate, lauryl acrylate, ethoxydiglycol acrylate, methoxytriglycol acrylate, phenoxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxy-3-phenoxyacrylate, neopentyl glycol diacrylate, 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate, trimethylolpropane acrylate, trimethylolpropane benzoate, methyl methacrylate, 2-ethylhexyl methacrylate, octadecyl methacrylate, cyclohexyl methacrylate, tetrahydrofurfuryl methacrylate phenoxyethyl methacrylate, methoxypolyethylene methacrylate, 2-hydroxyethyl methacrylate, 2-hydroxybutyl methacrylate, heptadecafluorodecyl methacrylate, trifluoromethyl methacrylate, trifluoroethyl acrylate, hexafluoropropyl methacrylate, 1, 6-hexanediol dimethacrylate, trimethylolpropane trimethacrylate, glycerol dimethacrylate hexamethylene diisocyanate, ethylene glycol dimethacrylate, urethane acrylate, epoxy acrylate, melamine acrylate, benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, 2- ([ 1,1' -biphenyl ] -2-oxy) ethyl acrylate, phenoxybenzyl acrylate, 3-phenoxybenzyl-3- (1-naphthyl) acrylate, ethyl (2E) -3-hydroxy-2- (3-phenoxybenzyl) acrylate, phenyl methacrylate, biphenyl methacrylate, 2-nitrophenyl acrylate, 4-nitrophenyl acrylate, 2-nitrophenyl methacrylate, 4-nitrophenyl methacrylate, 2-nitrobenzyl methacrylate, 4-nitrobenzyl methacrylate, 2-chlorophenyl acrylate, 4-chlorophenyl acrylate, 2-chlorophenyl methacrylate, 4-chlorophenyl methacrylate, ethyl o-phenylphenol acrylate, phenol, biphenyl methacrylate, o-phenylphenol ethoxyacrylate, 1- (biphenyl-2-ylmethyl) -4-phenylpiperazine, 1- (biphenyl-2-ylmethyl) -4- (2-methoxyphenyl) piperazine, 1- (biphenyl-2-ethoxyphenyl) -4- (2-ethoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (2-isopropoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (3-methoxyphenyl) piperazine, at least one selected from the group consisting of 1- (biphenyl-2-ylmethyl) -4- (4-methoxyphenyl) piperazine and bisphenol-diacrylate.
According to an embodiment, the monomer may be 1 to 50 wt% of the metal oxide dispersion. When included in the range, dispersibility of the metal oxide can be improved, curability in subsequent processes can be improved, and a coating layer having a high refractive index and flexibility can be provided.
Preferably, the monomer may be 50 to 70 wt%, 60 to 70 wt%, 40 to 60 wt%, 50 to 60 wt%, or 40 to 50 wt% of the metal oxide dispersion.
According to an embodiment, when the surface modifier is included in the range, the metal oxide sol dispersion effectively disperses zirconia particles into the sol dispersion while maintaining a high refractive index, a suitably low viscosity for forming a thin film, and an effective light transmittance. Thus, even if the metal oxide dispersion liquid of the present invention is filled with zirconia particles at a high concentration, stable dispersibility can be ensured, and a metal oxide sol that maintains high transparency can be produced.
According to an embodiment, the surface modifier includes a silane coupling agent, which may be a silane including at least one selected from the group consisting of an acrylate group, (meth) acrylic group, epoxy group (epoxy group), alkoxy group (alkoxy), vinyl group (vinyl group), phenyl group (phenyl group), methacryloxy group (metacryloxy group), amino group (amino group), chlorosilane group (chlorosilane group), chloropropyl group (chloropropyl) and mercapto group (mercapto).
In accordance with one embodiment of the present invention, the surface modifier may include a surfactant selected from the group consisting of gamma-methacryloxypropyl trimethoxysilane, 4-aminobutyl methyl diethoxysilane, 3-aminopropyl trimethoxysilane, N-2-aminoethyl-3-aminopropyl diethyl isopropoxysilane, (mercaptomethyl) dimethylethoxysilane, di-4-mercaptobutyl dimethoxysilane, 3-mercaptopropyl triisopropoxysilane, 3-methacryloxypropyl dimethylethoxysilane, 3-acryloxypropyl trimethoxysilane, (3-glycidoxypropyl) methyldimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, 3-chloropropyltrimethoxysilane, 4-bromobutyl methyldibutoxysilane, 5-iodohexyl diethyl methoxysilane, 3-isocyanatopropyl trimethoxysilane, 3-isothiocyanatepropyl methyldimethoxysilane, 3-hydroxybutyl isopropyl dimethoxysilane, bis (2-hydroxyethyl) -3-aminopropyl triethoxysilane, bromophenyl trimethoxysilane, (2- (iodophenyl) ethyl) dimethoxysilane, bis (chlorophenyl) propyl trimethoxysilane, bis (dimethoxyphenyl) -bis (dimethoxypropyl) carbodiimide, N-dimethoxypropyl-carbodiimide, N- (dimethoxypropyl) -carbodiimide, N-propylmethoxy-silane, N- (iodophenyl) ethyl) dimethoxysilane, bis (2-hydroxyethyl) propyltrimethoxysilane, 3-thiomethyl) propyl- (2-propyltrimethoxysilane, 3-mercaptopropyl-propyltrimethoxysilane, and (2-propylthioethoxysilane At least one selected from the group consisting of 3- (trimethoxysilyl) propanol, (3, 5-hexanedione) triethoxysilane, 3- (trimethoxysilyl) propyl acetoacetate, 3- (trimethoxysilyl) propyl methacrylate silane, 3-aminopropyl trimethoxysilane, 2-aminopropyl trimethoxysilane, N- (2-aminoethyl) -3-aminopropyl methyldimethoxysilane, 3-ureidopropyl trimethoxysilane, N-ethoxycarbonyl-3-aminopropyl trimethoxysilane, N-triethoxysilylpropyl triethyltriamine, N-trimethoxysilylpropyl triethyltriamine, 10-trimethoxysilyl-1, 4, 7-triazoldecane, 10-triethoxysilyl-1, 4, 7-triazoldecane, 9-trimethoxysilyl-3, 6-azo-nonanoate, 3- (triethoxysilyl) propyl succinic anhydride, N-benzyl-3-aminopropyl trimethoxysilane, N-phenyl-3-aminopropyl trimethoxysilane, N-dioxyvinyl-3-aminopropyl trimethoxysilane and (methacryloyloxy) propyl trimethoxysilane.
According to an embodiment, the surface modifier may be 1 to 50 wt% of the metal oxide dispersion. When the surface modifier is less than 1 wt% in the metal oxide dispersion, the dispersibility of zirconia nanoparticles in the dispersion composition may be reduced, thereby generating a cloudiness phenomenon; when it exceeds 50% by weight, the silane compound is excessively bonded to the surface of the zirconia nanoparticles to cause inter-particle aggregation, which causes a problem of increasing the viscosity.
When the surface modifier is included in the above range, the dispersibility of the zirconia particles in the dispersion composition can be improved while the surface treatment reaction rate of the zirconia particles is properly maintained, and the problem of aggregation between the zirconia particles and eventually lowering of the dispersibility due to adhesion of the excessively added surface modifier to the zirconia particle surfaces can be effectively prevented.
According to an embodiment, the metal oxide dispersion liquid further includes a dispersant, which may include at least one selected from the group consisting of a polyether acid-based compound, a polyether amine-based compound, a polyether acid/amine mixture, an ester-based compound including a phosphoric acid group, and a polyether-based compound including a phosphoric acid group.
According to an embodiment, when the dispersant is less than 1 wt%, it may be difficult to be compatible with a resin composition composed of an organic compound in a subsequent process; when it exceeds 20% by weight, the dispersant may be excessively bonded to the zirconia particle surface, resulting in a decrease in refractive index.
According to an embodiment, the metal oxide dispersion may further include an organic solvent, which may be 30 to 50 wt% to aid in dispersion. The solvent may be (almost) completely removed for subsequent processing to form a solvent-free sol dispersion.
According to one embodiment, when the organic solvent is less than 30 wt% in the metal oxide dispersion, the dispersion, viscosity, and optical properties are affected by the fact that the minimum range functioning as a dispersion medium is not reached; when the amount exceeds 50% by weight, the solvent removal time is increased, which lowers the refractive index and brightness of an optical film made of the metal oxide dispersion, lowers the light transmittance of the cured film, and improves the haze.
According to one embodiment, the metal oxide dispersion may be solvent-free.
According to an embodiment, the viscosity of the metal oxide dispersion may be 200cP to 50,000cP. Preferably, the viscosity of the metal oxide dispersion may be 200cP to 40,000cP;200cP to 30,000cP;200cP to 20,000cP;200cP to 10,000cP;200cP to 5,000;200cP to 1,000cP;200cP to 500;1,000cP to 50,000cP;30,000cP to 50,000cP;20,000cP to 50,000cP;20,000cP to 40,000cP;20,000cP to 30,000cP;30,000cP to 50,000cP; or 40,000cp to 50,000cp, the metal oxide dispersion may be solvent-free, and may be a sol dispersion. When the viscosity is high, it is difficult to form a liquid with an organic material, and also the dispersibility of zirconia particles in the dispersion is reduced, and it is difficult to form a uniform film layer at the time of manufacturing a film, resulting in a decrease in optical properties. Viscosity can be measured using the DV2T LV spindle (manufactured by Brookfield). In addition, the viscosity may be measured at a temperature of 25℃and a shear rate of 1.0 (1/s).
According to an embodiment, the refractive index of the metal oxide dispersion may be 1.60 or 1.670 or more. This allows for better compatibility with the ingredients or compositions used in subsequent processes, resulting in a coating having high brightness efficiency, high light transmittance, and high refractive index.
According to one embodiment, the metal oxide dispersion may have a yellowness (Yellow Index; Y.I) of 30 or less and a Haze (Haze) of 20 or less.
The metal oxide dispersion according to an embodiment of the present invention includes zirconia nanoparticles having a crystal structure in which a mixing ratio is adjusted, whereby the full width at half maximum and the crystal size of the crystal structure can be determined according to the mixing ratio, and when the dispersion is mixed with a monomer of an acrylic ester having a high refractive index having the same content of zirconia, the yellowness in optical properties can be improved.
The thin film composition for a display according to another embodiment of the present invention includes the metal oxide dispersion liquid according to an embodiment of the present invention; a UV photoinitiator; and a UV curable monomer.
According to an embodiment, the UV photoinitiator may include a cationic photoinitiator, a radical photoinitiator, or both.
According to an embodiment, the UV photoinitiator may include at least any one selected from the group consisting of a cationic photoinitiator and a radical photoinitiator: wherein the cationic photoinitiator is selected from onium salts, diazonium salts, sulfonium salt compounds and imidazoles; the free radical photoinitiator is selected from thioxanthones, phosphites, triazines, benzophenones, benzoins, oximes, acetones, aminoketones, ketones, benzoin ether acetophenones, anthraquinones and aromatic phosphine oxides.
According to an embodiment, the UV photoinitiator may be 2 to 5 wt% of the film composition for display. When the UV photoinitiator is less than 2% by weight in the film composition for display, the film composition is not sufficiently cured, and thus it is difficult to obtain an appropriate hardness; when the amount exceeds 5% by weight, problems such as cracking and peeling may occur after film formation due to curing shrinkage.
According to an embodiment, the UV curable monomer may include an acrylate-based resin. The acrylic resin is a saturated hydrocarbon polymer having no double bond in the molecule, and has excellent oxidation resistance due to its inherent properties, and thus has excellent weather resistance.
According to an embodiment, the UV curable monomer may include at least one selected from the group consisting of glycidyl acrylate, glycidyl methacrylate, glycidyl- α -ethyl acrylate, glycidyl- α -n-propyl acrylate, glycidyl- α -butyl acrylate, 3, 4-epoxybutyl methacrylate, 3, 4-epoxybutyl acrylate, methyl 6, 7-epoxyheptyl methacrylate, 6, 7-epoxyheptyl acrylate, 6, 7-epoxyheptyl- α -ethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl methacrylate, tripropylene glycol diacrylate, dipropylene glycol diacrylate, 1, 6-hexanediol diacrylate, and trimethylolpropane triacrylate.
According to an embodiment, the film composition for a display of the present invention may further include an acrylic resin.
According to an embodiment, the acrylic resin may include at least any one selected from the group consisting of hydroxyethyl acrylate (HEA), hydroxyethyl methacrylate (HEMA), hexanediol diacrylate (HDDA), tripropylene glycol diacrylate (TPGDA), ethylene Glycol Diacrylate (EGDA), trimethylolpropane triacrylate (TMPTA), trimethylolpropane ethoxytriacrylate (TMPEOTA), glycerol Propoxylated Triacrylate (GPTA), pentaerythritol tetraacrylate (PETA), benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, 2- ([ 1,1' -biphenyl ] -2-oxy) ethyl acrylate, phenoxybenzyl acrylate, 3-phenoxybenzyl-3- (1-naphthyl) acrylate, phenyl methacrylate, biphenyl methacrylate, phenyl 2-nitroacrylate, phenyl 4-nitroacrylate, phenyl 2-nitromethacrylate, phenyl 4-nitromethacrylate, and dipentaerythritol hexaacrylate (DPHA).
The film composition according to an embodiment of the present invention has a high refractive index and can improve yellowing of the film.
An optical film according to still another embodiment of the present invention includes a cured product of the dispersion composition for a display according to an embodiment of the present invention.
According to one embodiment, a substrate is prepared, and a dispersion composition for a display according to an embodiment of the present invention is laminated or coated on the substrate to be UV-cured, thereby forming a coating layer to manufacture a cured product.
According to one embodiment, the optical film may include a substrate; and a coating (film, etc.) prepared from the dispersion composition for display of the present invention formed on at least a part of the substrate. In manufacturing the optical film, the metal oxide dispersion or the composition including the metal oxide dispersion may be formed into a coating layer in a state of only a trace amount of solvent or little solvent or no solvent in a process (free).
According to an embodiment, the substrate may be appropriately selected according to the use of the optical film, and may be a transparent substrate. The transparent substrate is not particularly limited as long as it is a transparent film. A film including a polyester fiber (polyester) such as polyethylene terephthalate (PET), polyethylene (ethylene vinyl acetate, EVA) or the like, a cycloolefin polymer (cyclic olefin polymer, COP), a cycloolefin copolymer (cyclic olefin copolymer, COC), a Polyacrylate (PAC), a Polycarbonate (PC), a Polyethylene (PE), a polymethyl methacrylate (PMMA), a polyether ether ketone (PEEK), a polyethylene naphthalate (PEI), a Polyimide (PI), a Triacetylcellulose (TAC), a methyl methacrylate (methyl methacrylate, MMA), a fluorine-based resin or the like, and an inorganic substrate having flexibility may be used.
According to an embodiment, the coating method may include at least any one selected from the group consisting of gravure coating, indirect gravure coating, 2 to 3 roll coating (roll pressure coating), 2 to 3 reverse roll coating (roll reverse coating), dip coating, 1 to 2 roll kiss coating, trailing blade coating (trailing balde coating), nip coating (nip coating), flexographic coating (flexographic coating), reverse blade coating (inverted knife coating), polished rod coating (polishing bar coating), and wire wound blade coating (wire wound doctor coating). After coating, the coating is cured by UV light, and the curing process is maintained for 10 seconds to 1 hour.
The diffusion film according to an embodiment of the present invention may be used for diffusion films required for backlight units of mobile phones, tablet computers, PDP, notebook computers, display screens, TV.
An optical element for a display according to still another embodiment of the present invention includes the diffusion film of an embodiment of the present invention.
According to an embodiment, the optical element for a display may be used as an optical element of a backlight unit of a mobile phone, a tablet computer, a PDP, a notebook computer, a display screen, a TV.
The present invention will be described in more detail with reference to examples and comparative examples.
However, the following examples are merely illustrative of the present invention, and the content of the present invention is not limited to the following examples.
Comparative example 1
The zirconia nanoparticles were synthesized by hydrothermal synthesis, and at this time, the synthesized zirconia particles had a mixed structure of tetragonal system and monoclinic system. In the crystal phase of the zirconia particles, the volume fraction of the tetragonal structure was 46.5%, the crystal size was 12.6nm, and the FWHM was 0.659. The volume fraction of monoclinic structure was 56.5%, the crystal size was 15.3nm, and the FWHM was 0.546.
The above-synthesized zirconia was mixed with 61wt%, a phosphoric acid-based dispersant was 5wt%, and an acrylic acid ester-based monomer was 34wt% to obtain a zirconia monomer dispersion.
Comparative example 2
In this case, the volume fraction of the tetragonal structure in the crystal phase of the zirconia particles was 53.1%, the crystal size was 11.7nm, and the FWHM was 0.710. The volume fraction of monoclinic structure was 46.9%, the crystal size was 15.4nm, and FWHM was 0.541.
A monomer dispersion was prepared in the same manner as in comparative example 1.
Comparative example 3
The zirconium oxide nano particles with a tetragonal system and monoclinic system mixed structure are synthesized by a hydrothermal synthesis method. At this time, in the crystal phase of the zirconia particles, the volume fraction of the tetragonal structure was 55.7%, the crystal size was 10.8nm, and the FWHM was 0.766. The volume fraction of monoclinic structure was 44.3%, the crystal size was 12.5nm, and the FWHM was 0.663.
A monomer dispersion was prepared in the same manner as in comparative example 1.
Example 1
The zirconium oxide nano particles with a tetragonal system and monoclinic system mixed structure are synthesized by a hydrothermal synthesis method. At this time, in the crystal phase of the zirconia particles, the volume fraction of the tetragonal structure was 60.2%, the crystal size was 7.8nm, and the FWHM was 0.980. The volume fraction of monoclinic structure was 39.8%, the crystal size was 9.9nm, and the FWHM was 0.712.
A monomer dispersion was prepared in the same manner as in comparative example 1.
Example 2
The zirconium oxide nano particles with a tetragonal system and monoclinic system mixed structure are synthesized by a hydrothermal synthesis method. At this time, in the crystal phase of the zirconia particles, the volume fraction of the tetragonal structure was 60.7%, the crystal size was 7.7nm, and the FWHM was 0.990. The volume fraction of monoclinic structure was 39.3%, the crystal size was 7.8nm, and the FWHM was 0.978.
A monomer dispersion was prepared in the same manner as in comparative example 1.
Example 3
The zirconium oxide nano particles with a tetragonal system and monoclinic system mixed structure are synthesized by a hydrothermal synthesis method. At this time, in the crystal phase of the zirconia particles, the volume fraction of the tetragonal structure was 62.5%, the crystal size was 7.3nm, and FWHM 1.042. The volume fraction of monoclinic structure was 37.5%, the crystal size was 9.9nm, and FWHM was 0.781.
A monomer dispersion was prepared in the same manner as in comparative example 1.
< refractive index measurement method >
The coating solution samples prepared according to this example were dropped to the prism at room temperature (25 ℃) and then the measurement was automatically started when the start key was pressed to reach the set temperature, and the measurement results were the refractive index of the composition as shown in table 1.
Measuring equipment, ATAGO/JAPAN
Model: RX-5000Alpha
Table 1 shows the full width at half maximum (FWHM), crystal size, volume fraction, refractive index of the dispersion, yellowness (Y.I) and haze according to the zirconia crystal structure of comparative examples 1 to 3, examples 1 to 3 of the present invention.
[ Table 1 ]
/>
Referring to table 1, the acrylic acid ester-monomer dispersions prepared according to examples 1 to 3 of the present invention have a volume fraction of the tetragonal system exceeding 60%, a volume fraction of the monoclinic system below 40%, and a crystal size below 10nm. Thus, the acrylic acid ester-monomer dispersions prepared in examples 1 to 3 of the present invention have a high refractive index of 1.690 to 1.695, while the yellowness (YI ASTM D1925) is reduced to less than 30, and at the same time, the effect of reducing haze can be confirmed.
In summary, the embodiments are illustrated by the limited figures, and a person of ordinary skill in the art can make various modifications and variations based on the description. Suitable results may be obtained if the techniques described are performed in a different order and/or if the components described are combined or combined in a different manner, or replaced or substituted by other components or equivalents.
Therefore, other embodiments, and the claims and their equivalents should be construed as included in the invention.
Claims (16)
1. A metal oxide dispersion liquid characterized in that,
comprising the following steps:
zirconia nanoparticles;
a monomer; and
The surface modifying agent is used for modifying the surface of the substrate,
the tetragonal full width at half maximum of the zirconia nanoparticle is 0.9 or more,
the full width at half maximum of the monoclinic system is 0.7 or more,
the crystal size of the zirconia nano particles is less than 10nm,
the volume fraction (Vm) of the monoclinic system calculated by the following formula 1 and formula 2 is 30% to 40%,
the tetragonal system volume fraction (Vt) calculated by the following equation 3 is 60% to 70%,
the zirconia nanoparticles are 40 wt% to 70 wt% of the metal oxide dispersion,
[ formula 1]
[ formula 2]
And
V m : volume fraction of monoclinic system
(111): for->(111) Monoclinic system strength of peak of plane
It (101): tetragonal strength of peak for (101) plane
[ formula 3]
Vt＝1-Vm
V t : volume fraction of tetragonal system.
2. The metal oxide dispersion according to claim 1, characterized in that,
the monomers include monomers selected from the group consisting of methyl acrylate, lauryl acrylate, ethoxydiglycol acrylate, methoxytriglycol acrylate, phenoxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, neopentyl glycol diacrylate, 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate, methyl methacrylate, 2-ethylhexyl methacrylate, octadecyl methacrylate, cyclohexyl methacrylate, tetrahydrofurfuryl methacrylate, phenoxyethyl methacrylate, 2-hydroxyethyl methacrylate, heptadecafluorodecyl methacrylate, trifluoromethyl methacrylate, trifluoroethyl acrylate, hexafluoropropyl methacrylate, 1, 6-hexanediol dimethacrylate, trimethylolpropane trimethacrylate, ethylene glycol dimethacrylate, urethane acrylate, epoxy acrylate, melamine acrylate, benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, ethyl 2- ([ 1,1' -biphenyl ] -2-oxo) acrylate, phenoxybenzyl acrylate, 3-phenoxybenzyl-3- (1-naphthyl) acrylate, ethyl (2E) -3-hydroxy-2- (3-phenoxybenzyl) acrylate, phenyl methacrylate, biphenyl methacrylate, at least one selected from the group consisting of 2-phenyl nitroacrylate, 4-phenyl nitromethacrylate, 2-nitrobenzyl methacrylate, 2-chlorophenyl acrylate, 4-chlorophenyl acrylate, 2-chlorophenyl methacrylate, phenol, 1- (biphenyl-2-ylmethyl) -4-phenylpiperazine, 1- (biphenyl-2-ylmethyl) -4- (2-methoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (2-ethoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (2-isopropoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (3-methoxyphenyl) piperazine, 1- (biphenyl-2-ylmethyl) -4- (4-methoxyphenyl) piperazine, and bisphenol diacrylate.
3. The metal oxide dispersion according to claim 1, characterized in that,
the monomer is 1 to 50 wt% of the metal oxide dispersion.
4. The metal oxide dispersion according to claim 1, characterized in that,
the surface modifying agent comprises a silane coupling agent,
the silane coupling agent is a silane comprising at least one selected from the group consisting of an acrylate group, (meth) acrylic group, epoxy group, alkoxy group, vinyl group, phenyl group, methacryloxy group, amino group, chlorosilane group, chloropropyl group, and mercapto group.
5. The metal oxide dispersion according to claim 1, characterized in that,
the surface modifier includes at least any one selected from the group consisting of gamma-methacryloxypropyl trimethoxysilane, 3-aminopropyl trimethoxysilane, 3-acryloxypropyl trimethoxysilane, (3-glycidoxypropyl) methyldimethoxy silane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, 3-chloropropyl trimethoxysilane, 3-isocyanatopropyl trimethoxysilane, 3-isothiocyanate propylmethyldimethoxy silane, bis (2-hydroxyethyl) -3-aminopropyl triethoxysilane, bromophenyl trimethoxysilane, 3- (trimethoxysilyl) propanol, 3-aminopropyl trimethoxysilane, 2-aminopropyl trimethoxysilane, N- (2-aminoethyl) -3-aminopropyl methyldimethoxy silane, 3-ureidopropyl trimethoxysilane, N-trimethoxysilylpropyl triethyltriamine, 3- (triethoxysilyl) propylsuccinic anhydride, N-phenyl-3-aminopropyl trimethoxysilane and (methacryloxy) propyltrimethoxysilane.
6. The metal oxide dispersion according to claim 1, characterized in that,
the surface modifier is 1 to 50 wt% of the metal oxide dispersion.
7. The metal oxide dispersion according to claim 1, characterized in that,
the metal oxide dispersion also includes a dispersant,
the dispersant includes at least one selected from the group consisting of a polyether acid-based compound, a polyether amine-based compound, a polyether acid/amine mixture, an ester-based compound including a phosphoric acid group, and a polyether-based compound including a phosphoric acid group.
8. The metal oxide dispersion according to claim 1, characterized in that,
the metal oxide dispersion is solvent-free.
9. The metal oxide dispersion according to claim 1, characterized in that,
the viscosity of the metal oxide dispersion is 200cP to 50,000cP.
10. The metal oxide dispersion according to claim 1, characterized in that,
the refractive index of the metal oxide dispersion is 1.60 or more.
11. The metal oxide dispersion according to claim 1, characterized in that,
the yellowness of the metal oxide dispersion is 30 or less,
Haze is 20% or less.
12. A film composition for a display, characterized in that,
comprising the following steps:
the metal oxide dispersion of claim 1;
a UV photoinitiator; and
UV curable monomers.
13. The thin film composition for a display according to claim 12, wherein,
the UV photoinitiator includes at least any one selected from the group consisting of a cationic photoinitiator and a radical photoinitiator,
wherein the cationic photoinitiator is selected from onium salts, diazonium salts, sulfonium salt compounds and imidazoles; the free radical photoinitiator is selected from thioxanthones, phosphites, triazines, benzophenones, benzoins, oximes, acetones, aminoketones, ketones, anthraquinones and aromatic phosphine oxide compounds.
14. The thin film composition for a display according to claim 12, wherein,
the UV curable monomer includes at least any one selected from the group consisting of glycidyl acrylate, glycidyl methacrylate, 3, 4-epoxybutyl acrylate, methyl 6, 7-epoxyheptyl methacrylate, 6, 7-epoxyheptyl acrylate, 6, 7-epoxyheptyl-alpha-ethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl methacrylate, tripropylene glycol diacrylate, dipropylene glycol diacrylate, 1, 6-hexanediol diacrylate and trimethylolpropane triacrylate.
15. An optical film comprising the cured product of the dispersion composition for a display according to claim 12.
16. An optical element for a display comprising the optical film of claim 15.
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| JP2007171555A (en) * | 2005-12-22 | 2007-07-05 | Sumitomo Osaka Cement Co Ltd | Hard coat film and optical functional film, optical lens and optical component |
| JP2010189506A (en) * | 2009-02-17 | 2010-09-02 | Dic Corp | Resin composition containing inorganic oxide fine particle and cured product obtained from the composition |
| JP2017025225A (en) * | 2015-07-23 | 2017-02-02 | 株式会社日本触媒 | Dispersion liquid |
| CN107001067A (en) * | 2014-12-12 | 2017-08-01 | Dic株式会社 | The manufacture method of inorganic microparticle-dispersed liquid, solidification compound and its solidfied material comprising the dispersion liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2007171555A (en) * | 2005-12-22 | 2007-07-05 | Sumitomo Osaka Cement Co Ltd | Hard coat film and optical functional film, optical lens and optical component |
| JP2010189506A (en) * | 2009-02-17 | 2010-09-02 | Dic Corp | Resin composition containing inorganic oxide fine particle and cured product obtained from the composition |
| CN107001067A (en) * | 2014-12-12 | 2017-08-01 | Dic株式会社 | The manufacture method of inorganic microparticle-dispersed liquid, solidification compound and its solidfied material comprising the dispersion liquid |
| JP2017025225A (en) * | 2015-07-23 | 2017-02-02 | 株式会社日本触媒 | Dispersion liquid |
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