JP5697964B2 - 光硬化性組成物並びにこれを用いた金属ナノ粒子分散膜及び導電性薄膜の製造方法 - Google Patents
光硬化性組成物並びにこれを用いた金属ナノ粒子分散膜及び導電性薄膜の製造方法 Download PDFInfo
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- JP5697964B2 JP5697964B2 JP2010281283A JP2010281283A JP5697964B2 JP 5697964 B2 JP5697964 B2 JP 5697964B2 JP 2010281283 A JP2010281283 A JP 2010281283A JP 2010281283 A JP2010281283 A JP 2010281283A JP 5697964 B2 JP5697964 B2 JP 5697964B2
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- 239000010408 film Substances 0.000 title claims description 81
- 239000000203 mixture Substances 0.000 title claims description 80
- 239000002082 metal nanoparticle Substances 0.000 title claims description 53
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 239000010409 thin film Substances 0.000 title claims description 11
- 239000000178 monomer Substances 0.000 claims description 49
- 229910052751 metal Inorganic materials 0.000 claims description 48
- 239000002184 metal Substances 0.000 claims description 48
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 33
- 150000002736 metal compounds Chemical class 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 22
- 125000000524 functional group Chemical group 0.000 claims description 20
- -1 alkali metal salt Chemical class 0.000 claims description 19
- 239000006185 dispersion Substances 0.000 claims description 16
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- 239000000758 substrate Substances 0.000 claims description 15
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- 239000002904 solvent Substances 0.000 claims description 13
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 10
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- 230000001678 irradiating effect Effects 0.000 claims description 9
- 229910021645 metal ion Inorganic materials 0.000 claims description 9
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- 150000003839 salts Chemical class 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 8
- 239000002798 polar solvent Substances 0.000 claims description 8
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- 239000004332 silver Substances 0.000 claims description 8
- 230000009467 reduction Effects 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052783 alkali metal Inorganic materials 0.000 claims description 6
- 150000004696 coordination complex Chemical class 0.000 claims description 6
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- 239000010949 copper Substances 0.000 claims description 6
- 125000001033 ether group Chemical group 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
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- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 125000001931 aliphatic group Chemical group 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 150000005846 sugar alcohols Polymers 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
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- 239000012046 mixed solvent Substances 0.000 claims description 3
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- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
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- 125000005702 oxyalkylene group Chemical group 0.000 claims description 2
- 239000003505 polymerization initiator Substances 0.000 claims 1
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- 238000000034 method Methods 0.000 description 23
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 16
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- 239000003999 initiator Substances 0.000 description 13
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- 229910001961 silver nitrate Inorganic materials 0.000 description 8
- 238000004220 aggregation Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 6
- 238000004132 cross linking Methods 0.000 description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
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- UJOBWOGCFQCDNV-UHFFFAOYSA-N 9H-carbazole Chemical compound C1=CC=C2C3=CC=CC=C3NC2=C1 UJOBWOGCFQCDNV-UHFFFAOYSA-N 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 4
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- 235000011187 glycerol Nutrition 0.000 description 4
- 125000005843 halogen group Chemical group 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 229920002284 Cellulose triacetate Polymers 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 3
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229940100890 silver compound Drugs 0.000 description 3
- 150000003379 silver compounds Chemical class 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 125000004434 sulfur atom Chemical group 0.000 description 3
- XMLYCEVDHLAQEL-UHFFFAOYSA-N 2-hydroxy-2-methyl-1-phenylpropan-1-one Chemical compound CC(C)(O)C(=O)C1=CC=CC=C1 XMLYCEVDHLAQEL-UHFFFAOYSA-N 0.000 description 2
- GNKZMNRKLCTJAY-UHFFFAOYSA-N 4'-Methylacetophenone Chemical compound CC(=O)C1=CC=C(C)C=C1 GNKZMNRKLCTJAY-UHFFFAOYSA-N 0.000 description 2
- NTPLXRHDUXRPNE-UHFFFAOYSA-N 4-methoxyacetophenone Chemical compound COC1=CC=C(C(C)=O)C=C1 NTPLXRHDUXRPNE-UHFFFAOYSA-N 0.000 description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
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- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 description 2
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- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
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- 125000003277 amino group Chemical group 0.000 description 2
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- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
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- 125000005842 heteroatom Chemical group 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- RYZCLUQMCYZBJQ-UHFFFAOYSA-H lead(2+);dicarbonate;dihydroxide Chemical compound [OH-].[OH-].[Pb+2].[Pb+2].[Pb+2].[O-]C([O-])=O.[O-]C([O-])=O RYZCLUQMCYZBJQ-UHFFFAOYSA-H 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
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- 229910052700 potassium Inorganic materials 0.000 description 2
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- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
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- 239000003021 water soluble solvent Substances 0.000 description 2
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- ZRIPJJWYODJTLH-UHFFFAOYSA-N (4-benzylphenyl)-(4-chlorophenyl)methanone Chemical compound C1=CC(Cl)=CC=C1C(=O)C(C=C1)=CC=C1CC1=CC=CC=C1 ZRIPJJWYODJTLH-UHFFFAOYSA-N 0.000 description 1
- WXPWZZHELZEVPO-UHFFFAOYSA-N (4-methylphenyl)-phenylmethanone Chemical compound C1=CC(C)=CC=C1C(=O)C1=CC=CC=C1 WXPWZZHELZEVPO-UHFFFAOYSA-N 0.000 description 1
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- JYAQYXOVOHJRCS-UHFFFAOYSA-N 1-(3-bromophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(Br)=C1 JYAQYXOVOHJRCS-UHFFFAOYSA-N 0.000 description 1
- SKBBQSLSGRSQAJ-UHFFFAOYSA-N 1-(4-acetylphenyl)ethanone Chemical compound CC(=O)C1=CC=C(C(C)=O)C=C1 SKBBQSLSGRSQAJ-UHFFFAOYSA-N 0.000 description 1
- HDMHXSCNTJQYOS-UHFFFAOYSA-N 1-(4-prop-2-enylphenyl)ethanone Chemical compound CC(=O)C1=CC=C(CC=C)C=C1 HDMHXSCNTJQYOS-UHFFFAOYSA-N 0.000 description 1
- BQTPKSBXMONSJI-UHFFFAOYSA-N 1-cyclohexylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1CCCCC1 BQTPKSBXMONSJI-UHFFFAOYSA-N 0.000 description 1
- HHVCCCZZVQMAMT-UHFFFAOYSA-N 1-hydroxy-3-phenylpyrrole-2,5-dione Chemical compound O=C1N(O)C(=O)C=C1C1=CC=CC=C1 HHVCCCZZVQMAMT-UHFFFAOYSA-N 0.000 description 1
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 description 1
- HIDBROSJWZYGSZ-UHFFFAOYSA-N 1-phenylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=CC=C1 HIDBROSJWZYGSZ-UHFFFAOYSA-N 0.000 description 1
- PIZHFBODNLEQBL-UHFFFAOYSA-N 2,2-diethoxy-1-phenylethanone Chemical compound CCOC(OCC)C(=O)C1=CC=CC=C1 PIZHFBODNLEQBL-UHFFFAOYSA-N 0.000 description 1
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 description 1
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 1
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 1
- DJCYDDALXPHSHR-UHFFFAOYSA-N 2-(2-propoxyethoxy)ethanol Chemical compound CCCOCCOCCO DJCYDDALXPHSHR-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- LCZVSXRMYJUNFX-UHFFFAOYSA-N 2-[2-(2-hydroxypropoxy)propoxy]propan-1-ol Chemical compound CC(O)COC(C)COC(C)CO LCZVSXRMYJUNFX-UHFFFAOYSA-N 0.000 description 1
- UHFFVFAKEGKNAQ-UHFFFAOYSA-N 2-benzyl-2-(dimethylamino)-1-(4-morpholin-4-ylphenyl)butan-1-one Chemical compound C=1C=C(N2CCOCC2)C=CC=1C(=O)C(CC)(N(C)C)CC1=CC=CC=C1 UHFFVFAKEGKNAQ-UHFFFAOYSA-N 0.000 description 1
- DZZAHLOABNWIFA-UHFFFAOYSA-N 2-butoxy-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(OCCCC)C(=O)C1=CC=CC=C1 DZZAHLOABNWIFA-UHFFFAOYSA-N 0.000 description 1
- ZCDADJXRUCOCJE-UHFFFAOYSA-N 2-chlorothioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(Cl)=CC=C3SC2=C1 ZCDADJXRUCOCJE-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- SVONRAPFKPVNKG-UHFFFAOYSA-N 2-ethoxyethyl acetate Chemical compound CCOCCOC(C)=O SVONRAPFKPVNKG-UHFFFAOYSA-N 0.000 description 1
- RSROEZYGRKHVMN-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;oxirane Chemical compound C1CO1.CCC(CO)(CO)CO RSROEZYGRKHVMN-UHFFFAOYSA-N 0.000 description 1
- CTHJQRHPNQEPAB-UHFFFAOYSA-N 2-methoxyethenylbenzene Chemical group COC=CC1=CC=CC=C1 CTHJQRHPNQEPAB-UHFFFAOYSA-N 0.000 description 1
- LWRBVKNFOYUCNP-UHFFFAOYSA-N 2-methyl-1-(4-methylsulfanylphenyl)-2-morpholin-4-ylpropan-1-one Chemical compound C1=CC(SC)=CC=C1C(=O)C(C)(C)N1CCOCC1 LWRBVKNFOYUCNP-UHFFFAOYSA-N 0.000 description 1
- XEEYSDHEOQHCDA-UHFFFAOYSA-N 2-methylprop-2-ene-1-sulfonic acid Chemical compound CC(=C)CS(O)(=O)=O XEEYSDHEOQHCDA-UHFFFAOYSA-N 0.000 description 1
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 description 1
- XLLXMBCBJGATSP-UHFFFAOYSA-N 2-phenylethenol Chemical group OC=CC1=CC=CC=C1 XLLXMBCBJGATSP-UHFFFAOYSA-N 0.000 description 1
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 description 1
- LEUJIOLEGDAICX-UHFFFAOYSA-N 3-chloroxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC=C(Cl)C=C3OC2=C1 LEUJIOLEGDAICX-UHFFFAOYSA-N 0.000 description 1
- KMSYDDGPKBBSNA-UHFFFAOYSA-N 3-ethyl-1-phenylpentan-1-one Chemical compound CCC(CC)CC(=O)C1=CC=CC=C1 KMSYDDGPKBBSNA-UHFFFAOYSA-N 0.000 description 1
- XSWGQBKLWYYSMY-UHFFFAOYSA-N 3-prop-2-enoylpyrrole-2,5-dione Chemical class C=CC(=O)C1=CC(=O)NC1=O XSWGQBKLWYYSMY-UHFFFAOYSA-N 0.000 description 1
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- 229920002799 BoPET Polymers 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 1
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- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 125000002485 formyl group Chemical group [H]C(*)=O 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical compound Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 description 1
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- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
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- FSPSELPMWGWDRY-UHFFFAOYSA-N m-Methylacetophenone Chemical compound CC(=O)C1=CC=CC(C)=C1 FSPSELPMWGWDRY-UHFFFAOYSA-N 0.000 description 1
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- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- JESXATFQYMPTNL-UHFFFAOYSA-N mono-hydroxyphenyl-ethylene Natural products OC1=CC=CC=C1C=C JESXATFQYMPTNL-UHFFFAOYSA-N 0.000 description 1
- 125000002757 morpholinyl group Chemical group 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
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- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
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- 238000005457 optimization Methods 0.000 description 1
- QUANRIQJNFHVEU-UHFFFAOYSA-N oxirane;propane-1,2,3-triol Chemical compound C1CO1.OCC(O)CO QUANRIQJNFHVEU-UHFFFAOYSA-N 0.000 description 1
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- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
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Description
とも以下の[A]〜[C]:
[A]還元により金属微粒子を生成可能な金属化合物
[B]金属化合物[A]を構成する金属イオン又は金属錯体と相互作用し、かつ、還元
により析出した金属微粒子の表面に吸着可能な官能基(Q)を有し、かつラジカル重
合性基を2以上有する多官能単量体
[C]光ラジカル重合開始剤
を含み、組成物中の多官能単量体[B]の配合量が、組成物の全量100質量%に対し53〜93質量%の範囲である光硬化性組成物。
化性組成物。
よび銅よりなる群から選択された少なくとも1種の金属の金属塩又は金属錯体である前
記[1]ないし[3]の何れかに記載の光硬化性組成物。
、カルボニル基、カルボキシル基及びカルボキシル基の塩から選択される1種又は2
種以上の官能基である前記[1]ないし[5]の何れかに記載の光硬化性組成物。
ないし[6]の何れかに記載の光硬化性組成物。
の何れかに記載の光硬化性組成物。
ネルギー線を照射することにより金属ナノ粒子の形成と硬化膜の形成とを一工程で行う
ことを特徴とする、金属ナノ粒子分散膜の製造方法。
エネルギー線を照射することにより硬化させて金属ナノ粒子分散膜を得る硬化工程と、
該金属ナノ粒子分散膜を焼成して基板上に導電性金属膜を形成させる焼成工程を含む導
電性薄膜の製造方法。
が挙げられる。
(1)ガラス瓶に、金属化合物[A]として50wt%に調整した硝酸銀水溶液0.5g、多官能単量体[B]としてポリエチレングリコールジアクリレート(n=14)(新中村化学株式会社製、商品名「A−600」)1g、開始剤[C]としてDC1173(チバスペシャルティケミカルズ社製、商品名「DAROCURE(ダロキュア)1173」)0.02gを取り、これらを混合して光硬化性組成物を調製した。得られた組成物は無色透明の液であった。この光硬化性組成物を、ガラス基板上にバーコーターを用いて塗布し、500mW/cm2の強度で15秒間紫外線を照射することによって硬化膜を得た。得られた硬化膜は濃黄色に呈色しており、銀のナノ粒子が生成していることが確認された。
後記表1に示す配合で、実施例1と同様にして光硬化性組成物を調製した。得られた組成物はいずれも無色透明の液であった。この光硬化性組成物を、ガラス基板上にバーコーターを用いて塗布し、紫外線を照射することによって硬化膜を得た。得られた硬化膜は、いずれも淡黄色から濃黄色に呈色しており、銀のナノ粒子が生成していることが確認された。また、得られた硬化膜を200℃、または300℃で45分間焼成したところ、銀白色〜金属光沢を有する焼成膜が得られた。焼成膜の導電性の評価結果を後記表1に示す。
実施例1において、A−600の量を0.5gとした以外は同様の配合により、光硬化性組成物を調製した。得られた組成物には、銀化合物の析出・沈降が見られた。調製直後の光硬化性組成物をガラス基板上にバーコーターを用いて塗布し、紫外線を照射することによって硬化膜を得たが、得られた硬化膜は黄褐色で亀裂やはがれが生じていた。
実施例1において、A−600の量を10gとした以外は同様の配合により、光硬化性組成物を調製した。得られた組成物は無色透明の液であった。この光硬化性組成物を、ガラス基板上にバーコーターを用いて塗布し、紫外線を照射することによって硬化膜を得た。得られた硬化膜は、薄い淡黄色を呈していた。得られた硬化膜を、酸素雰囲気中200℃または300℃で45分間焼成したところ、いずれの焼成膜も亀裂やはがれが生じており、導電性を示さなかった。
ガラス瓶に、単官能単量体[D]としてアクリル酸ナトリウム(40%中和)1gを投入し、これに金属化合物[A]として1mol/L塩化金酸水溶液0.5g、多官能単量体[B]としてポリエチレングリコールジアクリレート(n=14)(新中村化学株式会社製、商品名「A−600」)2g、開始剤[C]としてDC1173(チバスペシャルティケミカルズ社製、商品名「DAROCURE(ダロキュア)1173」)0.05gを加え、混合して光硬化性組成物を調製した。得られた組成物は淡黄色透明の液であった。この光硬化性組成物を、ガラス基板上にバーコーターを用いて塗布し、紫外線を照射することによって硬化膜を得た。得られた硬化膜は赤色に呈色しており、金のナノ粒子が生成していることが確認された。
Claims (11)
- 金属ナノ粒子分散膜を製造するために用いられる光硬化性組成物であって、少なくとも以下の[A]、[B]、[C]および[E]:
[A]還元により金属微粒子を生成可能な金属化合物
[B]金属化合物[A]を構成する金属イオン又は金属錯体と相互作用し、かつ、還
元により析出した金属微粒子の表面に吸着可能な官能基(Q)としてヒドロキシル
基、エーテル基、カルボニル基、カルボキシル基及びカルボキシル基の塩から選択
される官能基を有し、かつラジカル重合性基を2以上有する多官能単量体
[C]光ラジカル重合開始剤
[E]溶媒として水又は水と極性溶媒とを組み合わせた混合溶媒
を含み、組成物中の多官能単量体[B]の配合量が、組成物の全量100質量%に対し
53〜93質量%の範囲である光硬化性組成物。 - 前記金属化合物[A]が、水溶液の状態で添加されたものである請求項1記載の光硬化性組成物。
- 水分量が20質量%以下である請求項1又は2記載の光硬化性組成物。
- 前記金属化合物[A]が、鉄、コバルト、ニッケル、パラジウム、白金、金、銀および銅よりなる群から選択された少なくとも1種の金属の金属塩又は金属錯体である請求項1〜3のいずれか1項に記載の光硬化性組成物。
- 前記多官能単量体[B]が、前記官能基(Q)としてヒドロキシル基、エーテル基、カルボニル基、カルボキシル基及びカルボキシル基の塩から選択される官能基を有し、かつ前記ラジカル重合性基として2以上の(メタ)アクリロイル基を有する多官能(メタ)アクリル酸エステルである請求項1〜4のいずれか1項に記載の光硬化性組成物。
- 前記多官能単量体[B]のエーテル基がオキシアルキレン基である請求項1〜5のいずれか1項に記載の光硬化性組成物。
- 前記多官能単量体[B]が、ポリエチレングリコールジ(メタ)アクリレート及びポリプロピレングリコールジ(メタ)アクリレートから選択される1種又は2種以上のグリコール系ジ(メタ)アクリレートである請求項1〜4のいずれか1項に記載の光硬化性組成物。
- さらに、(メタ)アクリル酸および(メタ)アクリル酸のアルカリ金属塩から選択されるラジカル重合性の単官能単量体[D]を含有する請求項1〜7のいずれか1項に記載の光硬化性組成物。
- 前記溶媒[E]において、極性溶媒が、アルコール類、脂肪族多価アルコール類、ピロリドン類からなる群から選択された少なくとも一種である請求項1〜8のいずれか1項に記載の光硬化性組成物。
- 請求項1〜9の何れか1項記載の光硬化性組成物を基板に塗布し、活性エネルギー線を照射することにより金属ナノ粒子の形成と硬化膜の形成とを一工程で行うことを特徴とする、金属ナノ粒子分散膜の製造方法。
- 請求項1〜9の何れか1項記載の光硬化性組成物を基板に塗布し、活性エネルギー線を照射することにより硬化させて金属ナノ粒子分散膜を得る硬化工程と、該金属ナノ粒子分散膜を焼成して基板上に導電性金属膜を形成させる焼成工程を含む導電性薄膜の製造方法。
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