CN115710438A - 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
- CN115710438A CN115710438A CN202211005154.0A CN202211005154A CN115710438A CN 115710438 A CN115710438 A CN 115710438A CN 202211005154 A CN202211005154 A CN 202211005154A CN 115710438 A CN115710438 A CN 115710438A
- Authority
- CN
- China
- Prior art keywords
- metal oxide
- acrylate
- oxide dispersion
- group
- methacrylate
- 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
Links
- 239000006185 dispersion Substances 0.000 title claims abstract description 97
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 77
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 77
- 239000000203 mixture Substances 0.000 title claims abstract description 34
- 230000003287 optical effect Effects 0.000 title claims abstract description 17
- 239000010409 thin film Substances 0.000 title 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 34
- 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 55
- -1 methacryloxy group Chemical group 0.000 claims description 52
- 239000007788 liquid Substances 0.000 claims description 26
- 239000010408 film Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 19
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 17
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 9
- 229920000570 polyether Polymers 0.000 claims description 9
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical group CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-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
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 8
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 7
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 7
- 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 7
- 239000012952 cationic photoinitiator Substances 0.000 claims description 7
- 238000009792 diffusion process Methods 0.000 claims description 7
- 239000012788 optical film Substances 0.000 claims description 7
- 229910000077 silane Inorganic materials 0.000 claims description 7
- 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 7
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- CYKONRWVCOIAHL-UHFFFAOYSA-N 5-(oxiran-2-yl)pentyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCC1CO1 CYKONRWVCOIAHL-UHFFFAOYSA-N 0.000 claims description 6
- 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 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 6
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 6
- 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 5
- 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 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
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 claims description 5
- 125000003545 alkoxy group Chemical group 0.000 claims description 4
- 239000012949 free radical photoinitiator Substances 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
- 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
- SIADNYSYTSORRE-UHFFFAOYSA-N (4-chlorophenyl) 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=C(Cl)C=C1 SIADNYSYTSORRE-UHFFFAOYSA-N 0.000 claims description 3
- ARWSNPDINLVISQ-UHFFFAOYSA-N (4-nitrophenyl)methyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC1=CC=C([N+]([O-])=O)C=C1 ARWSNPDINLVISQ-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
- 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 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
- PTBAHIRKWPUZAM-UHFFFAOYSA-N 2-(oxiran-2-yl)ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCC1CO1 PTBAHIRKWPUZAM-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
- 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
- CYXODUIWJAVDAK-UHFFFAOYSA-N 3-(oxiran-2-yl)propyl prop-2-enoate Chemical compound C=CC(=O)OCCCC1CO1 CYXODUIWJAVDAK-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
- JSOZORWBKQSQCJ-UHFFFAOYSA-N 3-[ethoxy(dimethyl)silyl]propyl 2-methylprop-2-enoate Chemical compound CCO[Si](C)(C)CCCOC(=O)C(C)=C JSOZORWBKQSQCJ-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
- BIGOJJYDFLNSGB-UHFFFAOYSA-N 3-isocyanopropyl(trimethoxy)silane Chemical group CO[Si](OC)(OC)CCC[N+]#[C-] BIGOJJYDFLNSGB-UHFFFAOYSA-N 0.000 claims description 3
- YSEQJKPADSUILR-UHFFFAOYSA-N 3-isothiocyanatopropyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)CCCN=C=S YSEQJKPADSUILR-UHFFFAOYSA-N 0.000 claims description 3
- CJUFQURUUZMUOG-UHFFFAOYSA-N 3-tri(propan-2-yloxy)silylpropane-1-thiol Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)CCCS CJUFQURUUZMUOG-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
- WQZMWDXLSUFOEM-UHFFFAOYSA-N 4-(oxiran-2-yl)butyl prop-2-enoate Chemical compound C=CC(=O)OCCCCC1CO1 WQZMWDXLSUFOEM-UHFFFAOYSA-N 0.000 claims description 3
- YHFFINXFNYQPQA-UHFFFAOYSA-N 4-[diethoxy(methyl)silyl]butan-1-amine Chemical compound CCO[Si](C)(OCC)CCCCN YHFFINXFNYQPQA-UHFFFAOYSA-N 0.000 claims description 3
- ZPXLLRDCVGRHSX-UHFFFAOYSA-N 4-bromobutyl-dibutoxy-methylsilane Chemical compound CCCCO[Si](C)(CCCCBr)OCCCC ZPXLLRDCVGRHSX-UHFFFAOYSA-N 0.000 claims description 3
- 229930185605 Bisphenol Natural products 0.000 claims description 3
- UHISHDMZOCAXAG-UHFFFAOYSA-N C(C=C)(=O)OC1=C(C(=CC=C1)CC)C1=CC=CC=C1 Chemical compound C(C=C)(=O)OC1=C(C(=CC=C1)CC)C1=CC=CC=C1 UHISHDMZOCAXAG-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
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical class NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- KFXKOQKIAJLZNS-UHFFFAOYSA-N [ethoxy(dimethyl)silyl]methanethiol Chemical compound CCO[Si](C)(C)CS KFXKOQKIAJLZNS-UHFFFAOYSA-N 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 125000003277 amino group Chemical group 0.000 claims description 3
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims description 3
- CFFSNLWMOZUQEC-UHFFFAOYSA-N bis[2-(chloromethyl)phenyl]-dimethoxysilane Chemical compound C=1C=CC=C(CCl)C=1[Si](OC)(OC)C1=CC=CC=C1CCl CFFSNLWMOZUQEC-UHFFFAOYSA-N 0.000 claims description 3
- OOTYXUYBOQGTCY-UHFFFAOYSA-N bromomethyl-dimethoxy-phenylsilane Chemical compound CO[Si](CBr)(OC)C1=CC=CC=C1 OOTYXUYBOQGTCY-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
- ICAWDVNMIVLRFZ-UHFFFAOYSA-N diethyl-(5-iodohexyl)-methoxysilane Chemical compound CC[Si](CC)(OC)CCCCC(C)I ICAWDVNMIVLRFZ-UHFFFAOYSA-N 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
- 125000003700 epoxy group Chemical group 0.000 claims description 3
- MHBPZEDIFIPGSX-UHFFFAOYSA-N ethyl n-(3-trimethoxysilylpropyl)carbamate Chemical compound CCOC(=O)NCCC[Si](OC)(OC)OC MHBPZEDIFIPGSX-UHFFFAOYSA-N 0.000 claims description 3
- JOXVFLZWHLAZIM-UHFFFAOYSA-N ethyl prop-2-eneperoxoate;2-phenylphenol Chemical compound CCOOC(=O)C=C.OC1=CC=CC=C1C1=CC=CC=C1 JOXVFLZWHLAZIM-UHFFFAOYSA-N 0.000 claims description 3
- PWGCTKVAPNBAFV-UHFFFAOYSA-N ethyl-[2-(2-iodophenyl)ethyl]-dimethoxysilane Chemical compound CC[Si](OC)(OC)CCC1=CC=CC=C1I PWGCTKVAPNBAFV-UHFFFAOYSA-N 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
- 150000002460 imidazoles Chemical class 0.000 claims description 3
- LEIOXRUNQWHHCT-UHFFFAOYSA-N n'-[3-[diethyl(propan-2-yloxy)silyl]propyl]ethane-1,2-diamine Chemical compound CC(C)O[Si](CC)(CC)CCCNCCN LEIOXRUNQWHHCT-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
- CLYWMXVFAMGARU-UHFFFAOYSA-N n-benzyl-3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCNCC1=CC=CC=C1 CLYWMXVFAMGARU-UHFFFAOYSA-N 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
- FSDNTQSJGHSJBG-UHFFFAOYSA-N piperidine-4-carbonitrile Chemical compound N#CC1CCNCC1 FSDNTQSJGHSJBG-UHFFFAOYSA-N 0.000 claims description 3
- KRIOVPPHQSLHCZ-UHFFFAOYSA-N propiophenone Chemical class CCC(=O)C1=CC=CC=C1 KRIOVPPHQSLHCZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000003254 radicals Chemical class 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
- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical group C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-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
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 238000003848 UV Light-Curing Methods 0.000 claims description 2
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical class C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims description 2
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- ZFFYKWNFIPKDLY-UHFFFAOYSA-N phenyl 2-nitroprop-2-enoate Chemical compound [O-][N+](=O)C(=C)C(=O)OC1=CC=CC=C1 ZFFYKWNFIPKDLY-UHFFFAOYSA-N 0.000 claims 1
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
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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, the metal oxide dispersion according to an embodiment of the invention includes zirconia nanoparticles; a monomer; and a surface modifier, wherein the tetragonal full width at half maximum (FWHM) of the zirconia nanoparticles is 0.9 or more, and the monoclinic full width at half maximum is 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 by polymer materials, and therefore methods of mixing and dispersing metal oxide particles having a high refractive index into a polymer have been actively developed.
In order to realize the performance of a display such as high luminance, high contrast, and low power consumption, an organic-inorganic hybrid material having metal oxide particles with a high refractive index is used as a transparent material for a display, and is expected to be widely used in the future.
However, although the organic-inorganic hybrid material having the metal oxide particles with a high refractive index can increase the refractive index by the metal oxide particles, it simultaneously decreases optical properties such as light transmittance, haze (haze), and yellowness (yellow index), and is limited in use as a display material.
In order to solve this problem, many techniques have been studied to improve yellowness while maintaining physical properties such as refractive index and viscosity, and these techniques generally change the synthetic method of inorganic substances or use a large amount of additives, which has a problem of affecting other physical properties.
Therefore, there is a need for a technique for preparing a dispersion of metal oxide particles that can improve the yellowness of an organic-inorganic hybrid material having highly refractive metal oxide particles without affecting other physical properties.
The above background is the content of the present invention grasped or learned by the inventors during the development of the present invention, and should not be construed as necessarily being the commonly known technology disclosed before the present invention is applied.
Disclosure of Invention
Problems to be solved by the invention
The present invention has been made to solve the above problems, and provides a metal oxide dispersion, a thin film composition for a display, and an optical element for a display, which can realize a high refractive index and a low yellowness by adjusting a crystal phase mixing ratio of zirconia nanoparticles.
The technical problems to be solved by the present invention are not limited to the above-mentioned problems, and other problems not mentioned will be clearly understood by those skilled in the art from the following description.
Means for solving the problems
The metal oxide dispersion liquid according to an embodiment of the present invention may include: zirconia nanoparticles; a monomer; and a surface modifier, wherein the zirconia nanoparticles have a full width at half maximum (FWHM) of 0.9 or more in the tetragonal system and a full width at half maximum (FWHM) of 0.7 or more in the monoclinic system.
According to an embodiment, the crystal size of the zirconia nanoparticles may be 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 volume fraction (Vt) of the tetragonal system calculated by the following equation 3 may be 60% to 70%:
[ equation 1]
[ equation 2]
V m : volume fraction of monoclinic system
It (101): tetragonal intensity 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 to 70 wt% in the metal oxide dispersion.
According to one embodiment of the method of manufacturing the solar cell panel, the monomer may include a monomer selected from the group consisting of methyl acrylate, lauryl acrylate, ethoxydiglycol acrylate, methoxytriethylene glycol acrylate, phenoxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxy-3-phenoxy acrylate, neopentyl glycol diacrylate, 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate, trimethylolpropane acrylate benzoate, trimethylolpropane benzoate, methyl methacrylate, 2-ethylhexyl methacrylate, octadecyl methacrylate, cyclohexyl methacrylate, tetrahydrofurfuryl acrylate, and mixtures thereof 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-biphenyl acrylate, ethyl 2- ([ 1,1' -biphenyl ] -2-oxy) acrylate, phenoxybenzyl methacrylate, and mixtures thereof, 3-phenoxybenzyl-3- (1-naphthyl) acrylate, ethyl (2E) -3-hydroxy-2- (3-phenoxybenzyl) acrylate, phenyl methacrylate, diphenyl methacrylate, 2-phenyl nitroacrylate, 4-phenyl nitroacrylate, 2-phenyl nitromethacrylate, 4-phenyl nitromethacrylate, 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 ethoxy acrylate, 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.
According to an embodiment, the monomer may be 1 to 50% by weight in the metal oxide dispersion liquid.
According to an embodiment, the surface modifier may include a silane coupling agent, and the silane coupling agent may be a silane including at least one selected from the group consisting of an acrylate group, a (meth) acrylate group, an epoxy group, an alkoxy group, a vinyl group, a phenyl group, a methacryloxy group, an amino group, a chlorosilyl group, a chloropropyl group, and a mercapto group (mercapto).
According to one embodiment of the method of manufacturing the solar cell panel, the surface modifier may be selected from the group consisting of gamma-methacryloxypropyltrimethoxysilane, 4-aminobutylmethyldiethoxysilane, 3-aminopropyltrimethoxysilane, N-2-aminoethyl-3-aminopropyldiethylisopropoxysilane, (mercaptomethyl) dimethylethoxysilane, di-4-mercaptobutyldimethoxysilane, 3-mercaptopropyltriisopropoxysilane, 3-methacryloxypropyldimethylethoxysilane, 3-acryloxypropyltrimethoxysilane, (3-glycidoxypropyl) methyldimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, 3-chloropropyltrimethoxysilane, 4-bromobutylmethyldibutoxysilane, 5-iodohexyldiethylmethoxysilane, 3-isocyanatopropyltrimethoxysilane, 3-isothiocyanatopropylmethyldimethoxysilane, 3-hydroxybutylsopropyldimethoxysilane, bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane, bromophenyltrimethoxysilane, (2- (iodophenyl) ethyl) ethyldimethoxysilane, bis (chloromethylphenyl) dimethoxysilane, bromomethylphenyldimethoxysilane, bis (N-dimethoxypropylethoxysilane, N- (N-dimethoxyethyl) -carbodiimide, 3- (trimethoxysilyl) propanol, (3, 5-hexanedione) triethoxysilane, 3- (trimethoxysilyl) propylacetoacetate, 3- (trimethoxysilyl) propylmethacrylate silane, 3-aminopropyltrimethoxysilane, 2-aminopropyltrimethoxysilane, N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane, 3-ureidopropyltrimethoxysilane, N-ethoxycarbonyl-3-aminopropyltrimethoxysilane, N-triethoxysilylpropyltriethylenetriamine, N-trimethoxysilylpropyltriethylenetriamine, 10-trimethoxysilyl-1, 4, 7-triazoldecane, 10-triethoxysilyl-1, 4, 7-triazoldecane, 9-trimethoxysilyl-3, 6-azononanoate, 3- (triethoxysilyl) propylsuccinic anhydride, N-benzyl-3-aminopropyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, N-bisoxyethylene-3-aminopropyltrimethoxysilane and (methacryloxypropyltrimethoxysilane).
According to an embodiment, the surface modifier may be 1 to 50% by weight in 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 compound, a polyether amine compound, a polyether acid/amine mixture, an ester compound including a phosphoric acid group, and a polyether 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 an 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 onium salts, diazonium salts, sulfonium salt compounds, and imidazoles; the free radical photoinitiator is selected from thioxanthone compounds, phosphorus compounds, triazine compounds, benzophenone compounds, benzoin compounds, oxime compounds, propiophenone compounds, aminoketone compounds, ketone compounds, benzoin ether acetophenone compounds, anthraquinone compounds and aromatic phosphine oxide compounds.
According to an embodiment, the UV curing monomer may include at least any 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, 6, 7-epoxyheptyl methyl 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 one 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 provided by the embodiment of the invention, the acrylate monomer mixed dispersion liquid with low yellowness and high refractive index is prepared by adjusting the volume fraction of the mixed crystal phase of the zirconia nanoparticles. The zirconia nanoparticles having a crystal structure with a mixing ratio adjusted can determine the full width at half maximum and the crystal size of the crystal structure based on the mixing ratio. The metal oxide dispersion has excellent dispersibility of zirconia particles, and has excellent fluidity and moldability due to low viscosity, and thus can be used as an element, i.e., a sol dispersion for a display device for improving the efficiency of the display device.
The diffusion film and the optical element for display according to an embodiment of the present invention 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, and a TV.
Drawings
Fig. 1 is a drawing illustrating a crystal structure and density of a general zirconia particle.
Fig. 2 is a drawing illustrating measurement of the crystal size of the 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 the scope of the claims of the present application is not limited to the following embodiments. All changes to the embodiments, and equivalents and alternatives thereof, are intended to be embraced within the scope of the invention.
The terminology used in the description presented herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope. Where not otherwise stated in the context, singular expressions include plural meanings. In the present specification, terms such as "including" or "having" are used to express that there are features, numbers, steps, operations, constituent elements, components, or combinations thereof described in the specification, and do not exclude the possibility that one or more other features, numbers, steps, operations, constituent elements, components, or combinations thereof exist or are additionally added.
All terms used herein, including technical or scientific terms, have the ordinary meaning as understood by one of ordinary skill in the art without further definition. Terms commonly used as dictionary definitions should be understood as meanings in the related art, and cannot be interpreted as idealised or over formalised meanings without being explicitly defined in the present specification.
In the description with reference to the drawings, the same components are denoted by the same reference numerals regardless of the reference numerals, and redundant description thereof is omitted. In describing the embodiments, when it is judged that detailed description on related well-known technologies may unnecessarily obscure the embodiments, detailed description thereof is omitted.
In addition, in describing the components of the embodiments, terms such as first, second, a, B, (a), and (B) may be used. These terms are only used to distinguish one constituent element from another constituent element, and are not used to limit the nature, order, and the like of the respective constituent elements.
When a component has a function common to that of one embodiment, the component will be described with the same name in other embodiments. When no example is mentioned, the description of one embodiment can be applied to the other embodiments, and detailed description thereof is omitted.
A metal oxide dispersion according to an embodiment of the present invention includes zirconia nanoparticles; a monomer; and a surface modifier, wherein the zirconia nanoparticles may have a full width at half maximum (FWHM) of 0.9 or more and a full width at half maximum of 0.7 or more.
Fig. 1 is a drawing illustrating a crystal structure and density of a general zirconia particle.
Referring to fig. 1, the conventional zirconia particles have 3 kinds of crystal phases such as monoclinic (monoclinic), tetragonal (tetragonal) and cubic (cubic) depending on a, b and c3 crystal axes forming crystals.
The monoclinic system crystal phase keeps a stable state till 1400K, the tetragonal system crystal phase is from 1170K to 2640K, the cubic system crystal phase is between higher temperature and melting point, and the theoretical density is shown in the attached drawing.
The metal oxide dispersion according to an embodiment of the present invention includes a structure in which a tetragonal system and a monoclinic system are mixed in a mixed crystal phase of nano zirconia.
The metal oxide dispersion liquid according to an embodiment of the present invention can provide a dispersion liquid having a low yellowness (y.i) and a high refractive index by adjusting the volume fractions of a tetragonal system (2 θ =30.119 °) and a monoclinic system (2 θ =28.217 °) in a mixed crystal phase of nano zirconia.
Fig. 2 is a drawing illustrating measurement of the crystal size of the crystal structure of zirconia nanoparticles according to an embodiment of the present invention.
According to an embodiment, the zirconia nanoparticle crystal size (crystallite size) is the average of all zirconia nanoparticles in the total metal oxide dispersion, as shown by the crystal size in fig. 2. A representative sample of the metal oxide dispersion can be collected and the crystal size of the zirconia nanoparticles measured using a Scanning Electron Microscope (SEM).
According to an embodiment, the crystal size of the zirconia nanoparticles may be less than 10nm. When D of the zirconia particles 50 When the average crystal size exceeds 10nm, scattering occurs or agglomeration or precipitation occurs, which leads to an unsatisfactory appearance of the coating and a decrease in refractive index.
According to an embodiment, the volume fraction (Vm) of the monoclinic system (2 θ =28.217 °) calculated by the following formulas 1 and 2 may be 30% to 40%; the volume fraction (Vt) of the tetragonal system (2 θ =30.119 °) calculated by the following equation 3 may be 60% to 70%.
[ equation 1]
[ formula 2]
V m : volume fraction of monoclinic system
It (101): tetragonal intensity of peak for (101) plane
[ formula 3]
Vt=1-Vm
V t : volume fraction of tetragonal system
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, it is possible to reduce yellowness while achieving a high refractive index.
According to an embodiment, the zirconia nanoparticles may be 40 to 70 wt% in the metal oxide dispersion. When less than 40% by weight in the metal oxide dispersion, the brightness of the curable composition may be reduced, which may reduce the optical characteristics of a cured film produced in a subsequent process; when the amount exceeds 70% by weight, the dispersion interval between the zirconia nanoparticles rapidly decreases, which causes a problem that the viscosity of the dispersion excessively increases and the zirconia nanoparticles aggregate together.
Preferably, the zirconia nanoparticles may be 50 to 70 wt%, 60 to 70 wt%, 40 to 60 wt%, 50 to 60 wt%, or 40 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, and derivatives in which methacrylate and/or acrylate substituents are introduced.
And, the molecules of the monomer are again substituted with at least one of hydroxyl, aliphatic ring and 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 monomer may include 1 to 6 functional acrylates, such as difunctional, trifunctional, and the like.
According to one embodiment of the method of manufacturing the solar cell panel, the monomer may include a monomer selected from the group consisting of methyl acrylate, lauryl acrylate, ethoxydiglycol acrylate, methoxytriethylene glycol acrylate, phenoxyethyl acrylate, tetrahydrofurfuryl acrylate, isobornyl acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxy-3-phenoxy acrylate, neopentyl glycol diacrylate, 1, 6-hexanediol diacrylate, trimethylolpropane triacrylate, pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate, trimethylolpropane acrylate benzoate, trimethylolpropane benzoate, methyl methacrylate, 2-ethylhexyl methacrylate, octadecyl methacrylate, cyclohexyl methacrylate, tetrahydrofurfuryl acrylate, and mixtures thereof phenoxyethyl methacrylate, methoxy polyethylene 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-biphenyl acrylate, ethyl 2- ([ 1,1' -biphenyl ] -2-oxy) acrylate, phenoxybenzyl methacrylate, and mixtures thereof, 3-phenoxybenzyl-3- (1-naphthyl) acrylate, ethyl (2E) -3-hydroxy-2- (3-phenoxybenzyl) acrylate, phenyl methacrylate, diphenyl methacrylate, 2-phenyl nitroacrylate, 4-phenyl nitroacrylate, 2-phenyl nitromethacrylate, 4-phenyl nitromethacrylate, 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 ethoxy acrylate, 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.
According to an embodiment, the monomer may be 1 to 50% by weight in the metal oxide dispersion liquid. When included within the range, the dispersibility of the metal oxide may be improved, the curing property in the subsequent process may be improved, and a coating layer having a high refractive index and flexibility may 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% in the metal oxide dispersion.
According to an embodiment, when the surface modifier is included in the range, the metal oxide sol dispersion effectively disperses the 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 when 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 maintaining high transparency can be prepared.
According to an embodiment, the surface modifier includes a silane coupling agent, and the silane coupling agent may be a silane including at least one selected from the group consisting of an acrylate group, a (meth) acrylate group, an epoxy group, an alkoxy group, a vinyl group, a phenyl group, a methacryloxy group, an amino group, a chlorosilyl group, a chloropropyl group, and a mercapto group (mercapto).
According to one embodiment, the surface modifier may include a compound selected from the group consisting of gamma-methacryloxypropyltrimethoxysilane, 4-aminobutylmethyldiethoxysilane, 3-aminopropyltrimethoxysilane, N-2-aminoethyl-3-aminopropyldiethylisopropoxysilane, (mercaptomethyl) dimethylethoxysilane, di-4-mercaptobutyldimethoxysilane, 3-mercaptopropyltriisopropoxysilane, 3-methacryloxypropyldimethylethoxysilane, 3-acryloxypropyltrimethoxysilane, (3-glycidoxypropyl) methyldimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, 3-chloropropyltrimethoxysilane, 4-bromobutylmethyldibutoxysilane, 5-iodohexyldiethylmethoxysilane, 3-isocyanatopropyltrimethoxysilane, 3-isothiocyanatopropylmethyldimethoxysilane, 3-hydroxybutylsopropyldimethoxysilane, bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane, bromophenyltrimethoxysilane, (2- (iodophenyl) ethyl) ethyldimethoxysilane, bis (chloromethylphenyl) dimethoxysilane, bromomethylphenyldimethoxysilane, bis (N-dimethoxypropyl) ethylcarbodiimide, N- (N-dimethoxyethyl) -carbodiimide, 3- (trimethoxysilyl) propanol, (3, 5-hexanedione) triethoxysilane, 3- (trimethoxysilyl) propylacetoacetate, 3- (trimethoxysilyl) propylmethacrylate silane, 3-aminopropyltrimethoxysilane, 2-aminopropyltrimethoxysilane, N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane, 3-ureidopropyltrimethoxysilane, N-ethoxycarbonyl-3-aminopropyltrimethoxysilane, N-triethoxysilylpropyltriethylenetriamine, N-trimethoxysilylpropyltriethylenetriamine, 10-trimethoxysilyl-1, 4, 7-triazoldecane, 10-triethoxysilyl-1, 4, 7-triazoldecane, 9-trimethoxysilyl-3, 6-azoacetic acid nonyl ester, 3- (triethoxysilyl) propylsuccinic anhydride, N-benzyl-3-aminopropyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, N-bisoxyethylene-3-aminopropyltrimethoxysilane and (methacryloxypropyl) trimethoxysilane.
According to an embodiment, the surface modifier may be 1 to 50% by weight in the metal oxide dispersion. When the surface modifier is less than 1% by weight in the metal oxide dispersion, the dispersibility of the zirconia nanoparticles in the dispersion composition may be reduced, thereby generating a white turbidity phenomenon; when it exceeds 50% by weight, inter-particle agglomeration may occur due to excessive bonding of the silane compound to the surface of the zirconia nanoparticles, which may cause a problem of increasing viscosity.
When the surface modifier is included in the range, the dispersibility of the zirconia particles in the dispersion composition can be improved while appropriately maintaining the surface treatment reaction rate of the zirconia particles, and the problem that the excessively added surface modifier adheres to the surfaces of the zirconia particles to cause agglomeration among the zirconia particles, and finally, the dispersibility is lowered can be effectively prevented.
According to an embodiment, the metal oxide dispersion liquid further includes a dispersant, and the dispersant may include at least one selected from the group consisting of a polyether acid compound, a polyether amine compound, a polyether acid/amine mixture, an ester compound including a phosphoric acid group, and a polyether compound including a phosphoric acid group.
According to an embodiment, when the dispersant is less than 1% by weight, 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 surface of the zirconia particles to cause a decrease in refractive index.
According to an embodiment, the metal oxide dispersion may further include an organic solvent, which facilitates the dispersion, and may be 30 to 50 wt%. For subsequent processing, the solvent can be (almost) completely removed to form a solventless sol dispersion.
According to an embodiment, when the organic solvent is less than 30% by weight in the metal oxide dispersion, the dispersibility, viscosity, and optical properties are affected because the minimum range to function as a dispersion medium is not reached; when the amount exceeds 50% by weight, the time for removing the solvent is increased, the refractive index and brightness of the optical film made of the metal oxide dispersion are decreased, the light transmittance of the cured film is decreased, and the haze is increased.
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 to reduce the dispersibility of zirconia particles in a dispersion, and it is difficult to form a uniform thin film layer when a thin film is produced, resulting in a reduction in optical properties. Viscosity can be measured using the DV2T LV spindle (manufactured by Brookfield). Further, 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 ingredients or compositions used in subsequent processes to form coatings with high brightness efficiency, high light transmittance, and high refractive index.
According to an 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 with a mixing ratio adjusted, whereby a full width at half maximum and a crystal size of the crystal structure can be determined according to the mixing ratio, and when the same content of zirconia is contained as a high refractive index acrylate-based monomer mixed dispersion, yellowness in optical properties can be improved.
A film composition for a display according to another embodiment of the present invention includes the metal oxide dispersion according to one embodiment of the present invention; a UV photoinitiator; and a UV curable monomer.
According to an embodiment, the UV photoinitiator may comprise a cationic photoinitiator, a free 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 thioxanthone, phosphorus, triazine, benzophenone, benzoin, oxime, propiophenone, aminoketone, ketone, benzoin ether acetophenone, anthraquinone and aromatic phosphine oxide compounds.
According to an embodiment, the UV photoinitiator may be 2 to 5% by weight in the film composition for display. When the UV photoinitiator is less than 2% by weight in the film composition for display, the film composition may not be sufficiently cured, and thus it is difficult to obtain appropriate hardness; when the amount exceeds 5% by weight, there may occur a problem of cracking, peeling or the like after film formation due to curing shrinkage.
According to an embodiment, the UV curable monomer may include an acrylate resin. The acrylate resin is a saturated hydrocarbon polymer without double bonds in the molecule, and has excellent weather resistance due to its inherent property of excellent oxidation resistance.
According to an embodiment, the UV-curable monomer may include at least any 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, 6, 7-epoxyheptyl methyl 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 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 ethoxy triacrylate (TMPEOTA), glycerol Propoxylate Triacrylate (GPTA), pentaerythritol tetraacrylate (PETA), benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, 2-biphenyl acrylate, ethyl 2- ([ 1,1' -biphenyl ] -2-oxy) acrylate, phenoxybenzyl acrylate, 3-phenoxybenzyl-3- (1-naphthyl) acrylate, phenyl methacrylate, biphenyl methacrylate, 2-nitrophenylacrylate, 4-nitrophenylacrylate, 2-nitrophenyl methacrylate, 4-nitrophenyl methacrylate, and dipentaerythritol hexaacrylate (DPHA).
The film composition provided by the embodiment of the invention has 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 one embodiment of the present invention.
According to one embodiment, a substrate is prepared, and the dispersion composition for a display according to one embodiment of the present invention is laminated or coated on the substrate to be UV-cured, thereby forming a coating layer to produce a cured product.
According to one embodiment, the optical film may include a substrate; and a coating layer (film, thin film, etc.) prepared from the dispersion composition for display of the present invention formed on at least a part of the substrate. In the production of the optical film, the metal oxide dispersion or the composition comprising the metal oxide dispersion may form a coating layer in a state of having only a slight amount of solvent or having almost no solvent or process solvent (free).
According to one embodiment, the substrate may be appropriately selected depending on 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. May be a polyester (polyester) such as polyethylene terephthalate (PET), a polyethylene (EVA) such as Ethylene Vinyl Acetate (EVA), a Cyclic Olefin Polymer (COP), a 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 (PEN), a Polyetherimide (PEI), a polyimide (polyimide, PI), a triacetyl cellulose (triacetate, TAC), a methyl methacrylate (methyl methacrylate), a Methyl Methacrylate (MMA), a fluorocarbon-based resin, or the like, and may be a film having flexibility without a fluorine-based resin.
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 press coating (roll pressing coating), 2 to 3 reverse roll coating (roll reverse coating), dip coating, 1 to 2 roll kiss coating, trailing blade coating (trailing bag coating), nip coating (nip coating), flexographic coating (flexible coating), reverse blade coating (inverted knife coating), polishing bar coating (polishing bar coating), and wire wound blade coating (wire wound blade 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 a diffusion film required for a backlight unit of a mobile phone, a tablet computer, a PDP, a notebook computer, a display screen, and a 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 below with reference to examples and comparative examples.
However, the following examples are only for illustrating the present invention, and the contents of the present invention are not limited to the following examples.
Comparative example 1
The zirconia nanoparticles are synthesized by a hydrothermal synthesis method, and in this case, the synthesized zirconia particles have 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 the monoclinic structure was 56.5%, the crystal size was 15.3nm, and the FWHM was 0.546.
The above-synthesized zirconium oxide was mixed with 61wt% of the phosphoric acid dispersant and 34wt% of the acrylic monomer to obtain a zirconium oxide monomer dispersion.
Comparative example 2
When zirconia nanoparticles having a mixed tetragonal and monoclinic structure were synthesized by hydrothermal synthesis, the volume fraction of the tetragonal structure was 53.1%, the crystal size was 11.7nm, and the FWHM was 0.710 in the crystal phase of the zirconia particles. The volume fraction of the monoclinic structure was 46.9%, the crystal size was 15.4nm, and the FWHM was 0.541.
The monomer dispersion was prepared in the same manner as in comparative example 1.
Comparative example 3
The zirconium oxide nano particles with a mixed structure of tetragonal system and monoclinic system 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 the monoclinic structure was 44.3%, the crystal size was 12.5nm, and the FWHM was 0.663.
The monomer dispersion was prepared in the same manner as in comparative example 1.
[ example 1]
The zirconium oxide nano particles with a mixed structure of tetragonal system and monoclinic system 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 the monoclinic structure was 39.8%, the crystal size was 9.9nm, and the FWHM was 0.712.
The monomer dispersion was prepared in the same manner as in comparative example 1.
[ example 2]
The zirconium oxide nanoparticles with a mixed tetragonal crystal structure and a monoclinic crystal 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 the monoclinic structure was 39.3%, the crystal size was 7.8nm, and the FWHM was 0.978.
The monomer dispersion was prepared in the same manner as in comparative example 1.
[ example 3]
The zirconium oxide nanoparticles with a mixed tetragonal crystal structure and a monoclinic crystal 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 the monoclinic structure was 37.5%, the crystal size was 9.9nm, and the FWHM was 0.781.
The monomer dispersion was prepared in the same manner as in comparative example 1.
< method of measuring refractive index >
A sample of the coating solution prepared according to this example was dropped at room temperature (25 ℃) to a prism, and then a start key was pressed to reach a set temperature to automatically start measurement, which was the refractive index of the composition, as shown in Table 1.
Measurement device ATAGO/JAPAN
The model is as follows: RX-5000Alpha
Table 1 shows full width at half maximum (FWHM) according to the crystal structure of zirconia, crystal size, volume fraction, refractive index of dispersion, yellowness (y.i) and haze of comparative examples 1 to 3, examples 1 to 3 of the present invention.
[ TABLE 1]
Referring to table 1, the acrylate-monomer dispersions prepared according to examples 1 to 3 of the present invention have a tetragonal system volume fraction of more than 60%, a monoclinic system volume fraction of less than 40%, and a crystal size of less than 10nm. Thus, the acrylate-monomer dispersions prepared in examples 1 to 3 of the present invention have a high refractive index of 1.690 to 1.695, and the yellowness (YI ASTM D1925) is reduced to less than 30, and the effect of reducing haze can be confirmed.
In summary, the embodiments have been described with reference to a limited number of figures, and those skilled in the art will be able to make numerous variations and modifications based on the description. Suitable results may also be achieved 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 by other components or equivalents.
Accordingly, other embodiments, other examples, and the scope of the claims and their equivalents should be construed to be included in the present invention.
Claims (19)
1. A metal oxide dispersion liquid characterized by comprising,
the method comprises the following steps:
zirconia nanoparticles;
a monomer; and
a surface-modifying agent, which is a mixture of a surfactant,
the full width at half maximum of the tetragonal system of the zirconia nanoparticles is 0.9 or more,
the full width at half maximum of the monoclinic system is 0.7 or more.
2. The metal oxide dispersion liquid according to claim 1,
the crystal size of the zirconia nanoparticles is less than 10nm.
3. The metal oxide dispersion liquid according to claim 1,
the volume fraction (Vm) of the monoclinic system calculated by the following equations 1 and 2 is 30% to 40%,
the volume fraction (Vt) of the tetragonal system calculated by the following equation 3 is 60% to 70%,
[ equation 1]
[ formula 2]
V m : volume fraction of monoclinic system
It (101): tetragonal intensity of peak for (101) plane
[ formula 3]
Vt=1-Vm
V t : volume fraction of tetragonal system.
4. The metal oxide dispersion liquid according to claim 1,
the zirconia nanoparticles are 40 to 70 weight percent of the metal oxide dispersion.
5. The metal oxide dispersion liquid according to claim 1,
<xnotran> , , , , , , , 2- , 2- , 2- -3- , ,1,6- , , , , , , , , 2- , , , , , , 2- , 2- , , , ,1,6- , , , , , , , , , , , , 2- , 2- ([ 1,1' - ] -2- ) , , 3- -3- (1- ) , </xnotran> At least one selected from the group consisting of ethyl (2E) -3-hydroxy-2- (3-phenoxybenzyl) acrylate, phenyl methacrylate, biphenyl methacrylate, phenyl 2-nitroacrylate, phenyl 4-nitroacrylate, phenyl 2-nitromethacrylate, phenyl 4-nitromethacrylate, 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 ethoxy acrylate, 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.
6. The metal oxide dispersion liquid according to claim 1,
the monomer is 1 to 50 wt% of the metal oxide dispersion.
7. The metal oxide dispersion liquid according to claim 1,
the surface modifying agent comprises a silane coupling agent,
the silane coupling agent is a silane including at least one selected from the group consisting of an acrylate group, a (meth) acrylate group, an epoxy group, an alkoxy group, a vinyl group, a phenyl group, a methacryloxy group, an amino group, a chlorosilyl group, a chloropropyl group, and a mercapto group.
8. The metal oxide dispersion liquid according to claim 1,
the surface modifier is selected from the group consisting of gamma-methacryloxypropyltrimethoxysilane, 4-aminobutylmethyldiethoxysilane, 3-aminopropyltrimethoxysilane, N-2-aminoethyl-3-aminopropyldiethylisopropoxysilane, (mercaptomethyl) dimethylethoxysilane, di-4-mercaptobutyldimethoxysilane, 3-mercaptopropyltriisopropoxysilane, 3-methacryloxypropyldimethylethoxysilane, 3-acryloxypropyltrimethoxysilane, (3-glycidoxypropyl) methyldimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, 3-chloropropyltrimethoxysilane, 4-bromobutylmethyldibutoxysilane, 5-iodohexyldiethylmethoxysilane, 3-isocyanatopropyltrimethoxysilane, 3-isothiocyanatopropylmethyldimethoxysilane, 3-hydroxybutylsopropyldimethoxysilane, bis (2-hydroxyethyl) -3-aminopropyltriethoxysilane, bromophenyltrimethoxysilane, (2- (iodophenyl) ethyl) ethyldimethoxysilane, bis (chloromethylphenyl) dimethoxysilane, bromomethylphenyldimethoxysilane, bis (N-dimethoxypropyldimethylsilyl) N- (3-dimethoxyethyl) iminosilane, N- (3-carbonylethoxypropyl) N-carbonylbismethoxysilane, N- (3-carbonylethoxypropyl) trimethoxysilane, 3-dimethoxysilane, 3-carbonyldimethoxysilane, N-carbonylpropyltrimethoxysilane, 3-dimethoxysilane, N-carbonyldimethylsiloxane, (3, 5-hexanedione) triethoxysilane, 3- (trimethoxysilyl) propylacetoacetate, 3- (trimethoxysilyl) propylmethacrylate silane, 3-aminopropyltrimethoxysilane, 2-aminopropyltrimethoxysilane, N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane, 3-ureidopropyltrimethoxysilane, N-ethoxycarbonyl-3-aminopropyltrimethoxysilane, N-triethoxysilylpropyltriethylenetriamine, N-trimethoxysilylpropyltriethylenetriamine, 10-trimethoxysilyl-1, 4, 7-triazoldecane, 10-triethoxysilyl-1, 4, 7-triazoldecane, 9-trimethoxysilyl-3, 6-azoacetic acid nonyl ester, 3- (triethoxysilyl) propylsuccinic anhydride, N-benzyl-3-aminopropyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, N-bisoxyethylene-3-aminopropyltrimethoxysilane, and (trimethoxyacryloxy) propyl.
9. The metal oxide dispersion liquid according to claim 1,
the surface modifier is 1 to 50 wt% of the metal oxide dispersion.
10. The metal oxide dispersion liquid according to claim 1,
the metal oxide dispersion liquid further includes a dispersant,
the dispersant includes at least one selected from the group consisting of a polyetheracid compound, a polyetheramine compound, a polyetheracid/amine mixture, an ester compound including a phosphoric acid group, and a polyether compound including a phosphoric acid group.
11. The metal oxide dispersion liquid according to claim 1,
the metal oxide dispersion is solvent-free.
12. The metal oxide dispersion liquid according to claim 1,
the viscosity of the metal oxide dispersion is 200cP to 50,000cP.
13. The metal oxide dispersion liquid according to claim 1,
the refractive index of the metal oxide dispersion is 1.60 or more.
14. The metal oxide dispersion liquid according to claim 1,
the yellowness of the metal oxide dispersion is 30 or less,
the haze is 20% or less.
15. A film composition for a display, characterized in that,
the method comprises the following steps:
the metal oxide dispersion liquid according to claim 1;
a UV photoinitiator; and
and (3) UV curing monomers.
16. The film composition for display use according to claim 15,
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 thioxanthone compounds, phosphorus compounds, triazine compounds, benzophenone compounds, benzoin compounds, oxime compounds, propiophenone compounds, aminoketone compounds, ketone compounds, benzoin ether acetophenone compounds, anthraquinone compounds and aromatic phosphine oxide compounds.
17. The film composition for display use according to claim 15,
the UV curable monomer includes at least any one selected from the group consisting of glycidyl acrylate, glycidyl methacrylate, glycidyl-alpha-ethyl acrylate, glycidyl-alpha-n-propyl acrylate, glycidyl-alpha-butyl acrylate, 3, 4-epoxybutyl methacrylate, 3, 4-epoxybutyl acrylate, 6, 7-epoxyheptyl methyl 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.
18. An optical film comprising a cured product of the dispersion composition for display use according to claim 15.
19. An optical element for display comprising the diffusion film according to claim 18.
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US20050200278A1 (en) * | 2003-09-12 | 2005-09-15 | Jones Clinton L. | Polymerizable compositions comprising nanoparticles |
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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US20050200278A1 (en) * | 2003-09-12 | 2005-09-15 | Jones Clinton L. | Polymerizable compositions comprising nanoparticles |
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 |
US20170342234A1 (en) * | 2014-12-12 | 2017-11-30 | Dic Corporation | Process for producing dispersion of fine inorganic particles, curable composition containing said dispersion, and cured object obtained therefrom |
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