TW201623467A - 光硬化性無電解鍍敷底塗劑 - Google Patents
光硬化性無電解鍍敷底塗劑 Download PDFInfo
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- TW201623467A TW201623467A TW104129603A TW104129603A TW201623467A TW 201623467 A TW201623467 A TW 201623467A TW 104129603 A TW104129603 A TW 104129603A TW 104129603 A TW104129603 A TW 104129603A TW 201623467 A TW201623467 A TW 201623467A
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- acrylate
- metal
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- 238000007772 electroless plating Methods 0.000 title claims abstract description 52
- 238000000016 photochemical curing Methods 0.000 title 1
- 229910052751 metal Inorganic materials 0.000 claims abstract description 112
- 239000002184 metal Substances 0.000 claims abstract description 112
- 150000001875 compounds Chemical class 0.000 claims abstract description 90
- 238000007747 plating Methods 0.000 claims abstract description 69
- 229920000587 hyperbranched polymer Polymers 0.000 claims abstract description 62
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 38
- 239000003999 initiator Substances 0.000 claims abstract description 13
- -1 acrylate compound Chemical class 0.000 claims description 137
- 239000000758 substrate Substances 0.000 claims description 65
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 40
- 239000010419 fine particle Substances 0.000 claims description 39
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 36
- JOYRKODLDBILNP-UHFFFAOYSA-N urethane group Chemical group NC(=O)OCC JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 27
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical group C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 25
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 claims description 25
- 125000000217 alkyl group Chemical group 0.000 claims description 24
- 125000004432 carbon atom Chemical group C* 0.000 claims description 24
- 239000010949 copper Substances 0.000 claims description 23
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- 229910052802 copper Inorganic materials 0.000 claims description 19
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 17
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 14
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 13
- 239000011859 microparticle Substances 0.000 claims description 13
- 229910052763 palladium Inorganic materials 0.000 claims description 13
- 125000006165 cyclic alkyl group Chemical group 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 11
- 239000011135 tin Substances 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 239000010931 gold Substances 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- 125000003545 alkoxy group Chemical group 0.000 claims description 6
- 125000002947 alkylene group Chemical group 0.000 claims description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 6
- 125000004093 cyano group Chemical group *C#N 0.000 claims description 6
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 6
- 229910052718 tin Inorganic materials 0.000 claims description 6
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- 150000001335 aliphatic alkanes Chemical group 0.000 claims description 4
- 125000003277 amino group Chemical group 0.000 claims description 4
- 150000001450 anions Chemical class 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims description 3
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 claims description 2
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 abstract description 7
- 239000002923 metal particle Substances 0.000 abstract description 2
- 229910001111 Fine metal Inorganic materials 0.000 abstract 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 141
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 71
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 53
- 239000000243 solution Substances 0.000 description 53
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 51
- 239000010408 film Substances 0.000 description 45
- 239000000126 substance Substances 0.000 description 43
- 239000002904 solvent Substances 0.000 description 41
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 38
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 34
- 229960004063 propylene glycol Drugs 0.000 description 34
- 235000013772 propylene glycol Nutrition 0.000 description 34
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 32
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 27
- 238000000034 method Methods 0.000 description 27
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 24
- 229920000642 polymer Polymers 0.000 description 24
- 238000006243 chemical reaction Methods 0.000 description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 21
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 18
- 239000002131 composite material Substances 0.000 description 18
- 150000002148 esters Chemical class 0.000 description 18
- 229910021645 metal ion Inorganic materials 0.000 description 18
- 239000000047 product Substances 0.000 description 17
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 16
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 16
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 16
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 15
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 150000003839 salts Chemical class 0.000 description 15
- 150000001412 amines Chemical class 0.000 description 14
- 125000001309 chloro group Chemical group Cl* 0.000 description 13
- 239000000203 mixture Substances 0.000 description 13
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 12
- 239000003638 chemical reducing agent Substances 0.000 description 12
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 12
- 125000005843 halogen group Chemical group 0.000 description 12
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 description 12
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 11
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- 229940042596 viscoat Drugs 0.000 description 10
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- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 9
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- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 9
- 239000011112 polyethylene naphthalate Substances 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
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- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 description 8
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- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical group CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 8
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
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- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 6
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- 229940035437 1,3-propanediol Drugs 0.000 description 6
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
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- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
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- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 6
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- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical group NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 description 5
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- 125000002723 alicyclic group Chemical group 0.000 description 3
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
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- OWBTYPJTUOEWEK-UHFFFAOYSA-N butane-2,3-diol Chemical compound CC(O)C(C)O OWBTYPJTUOEWEK-UHFFFAOYSA-N 0.000 description 3
- 238000001460 carbon-13 nuclear magnetic resonance spectrum Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000002508 contact lithography Methods 0.000 description 3
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 3
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- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 3
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- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 3
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- YNXCGLKMOXLBOD-UHFFFAOYSA-N oxolan-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CCCO1 YNXCGLKMOXLBOD-UHFFFAOYSA-N 0.000 description 1
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- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
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- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 1
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- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
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- 239000004417 polycarbonate Substances 0.000 description 1
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- 230000000379 polymerizing effect Effects 0.000 description 1
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- 238000007788 roughening Methods 0.000 description 1
- OJLCQGGSMYKWEK-UHFFFAOYSA-K ruthenium(3+);triacetate Chemical compound [Ru+3].CC([O-])=O.CC([O-])=O.CC([O-])=O OJLCQGGSMYKWEK-UHFFFAOYSA-K 0.000 description 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
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- 239000007787 solid Substances 0.000 description 1
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- 239000007858 starting material Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- AOCSUUGBCMTKJH-UHFFFAOYSA-N tert-butyl n-(2-aminoethyl)carbamate Chemical compound CC(C)(C)OC(=O)NCCN AOCSUUGBCMTKJH-UHFFFAOYSA-N 0.000 description 1
- POHWAQLZBIMPRN-UHFFFAOYSA-N tert-butyl n-(3-aminopropyl)carbamate Chemical compound CC(C)(C)OC(=O)NCCCN POHWAQLZBIMPRN-UHFFFAOYSA-N 0.000 description 1
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- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- JOUDBUYBGJYFFP-FOCLMDBBSA-N thioindigo Chemical compound S\1C2=CC=CC=C2C(=O)C/1=C1/C(=O)C2=CC=CC=C2S1 JOUDBUYBGJYFFP-FOCLMDBBSA-N 0.000 description 1
- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-UHFFFAOYSA-N 0.000 description 1
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 description 1
- 229960002447 thiram Drugs 0.000 description 1
- 229910001432 tin ion Inorganic materials 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 235000010487 tragacanth Nutrition 0.000 description 1
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- 229940116362 tragacanth Drugs 0.000 description 1
- PYHOFAHZHOBVGV-UHFFFAOYSA-N triazane Chemical compound NNN PYHOFAHZHOBVGV-UHFFFAOYSA-N 0.000 description 1
- IFXORIIYQORRMJ-UHFFFAOYSA-N tribenzylphosphane Chemical compound C=1C=CC=CC=1CP(CC=1C=CC=CC=1)CC1=CC=CC=C1 IFXORIIYQORRMJ-UHFFFAOYSA-N 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- TUQOTMZNTHZOKS-UHFFFAOYSA-N tributylphosphine Chemical compound CCCCP(CCCC)CCCC TUQOTMZNTHZOKS-UHFFFAOYSA-N 0.000 description 1
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 description 1
- WLPUWLXVBWGYMZ-UHFFFAOYSA-N tricyclohexylphosphine Chemical compound C1CCCCC1P(C1CCCCC1)C1CCCCC1 WLPUWLXVBWGYMZ-UHFFFAOYSA-N 0.000 description 1
- ABVVEAHYODGCLZ-UHFFFAOYSA-N tridecan-1-amine Chemical compound CCCCCCCCCCCCCN ABVVEAHYODGCLZ-UHFFFAOYSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- SWZDQOUHBYYPJD-UHFFFAOYSA-N tridodecylamine Chemical compound CCCCCCCCCCCCN(CCCCCCCCCCCC)CCCCCCCCCCCC SWZDQOUHBYYPJD-UHFFFAOYSA-N 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical group OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- 150000004072 triols Chemical class 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
- KCTAHLRCZMOTKM-UHFFFAOYSA-N tripropylphosphane Chemical compound CCCP(CCC)CCC KCTAHLRCZMOTKM-UHFFFAOYSA-N 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- QFKMMXYLAPZKIB-UHFFFAOYSA-N undecan-1-amine Chemical compound CCCCCCCCCCCN QFKMMXYLAPZKIB-UHFFFAOYSA-N 0.000 description 1
- 150000003673 urethanes Chemical class 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/0047—Photosensitive materials characterised by additives for obtaining a metallic or ceramic pattern, e.g. by firing
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
-
- 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
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
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Abstract
本發明的課題為提供一種注重環境,以少數步驟數可簡便處理,且得到充分基板密著性,作為無電解鍍敷之前處理步驟使用之新穎無電解鍍敷底塗劑。
本發明的解決手段為一種光硬化性底塗劑,其係於基材上藉由無電解鍍敷處理,用以形成金屬鍍敷膜之底塗劑,其係包含:(a)於分子末端具有銨基且重量平均分子量為1,000~5,000,000之超枝化聚合物(Hyperbranched polymer)、(b)金屬微粒子、(c)具有(甲基)丙烯醯基之聚合性化合物、及(d)光聚合起始劑。
Description
本發明係關於無電解鍍敷底塗劑,更詳細而言係關於光硬化性無電解鍍敷底塗劑。
由於無電解鍍敷僅將基材浸漬於鍍敷液,可得到與基材之種類或形狀無關且厚度均勻之被膜,亦可於塑膠或陶瓷、玻璃等之非導體材料形成金屬鍍敷膜,例如在汽車零件等之對樹脂成形體的高級感或美觀的賦予之類的裝飾用途、或電磁屏蔽、印刷基板及大規模積體電路等之配線技術等各種領域被廣泛使用。
通常,藉由無電解鍍敷而於基材(被鍍敷體)上形成金屬鍍敷膜時,進行用以提高基材與金屬鍍敷膜的密著性之前處理。具體而言,首先藉由各種蝕刻手段將被處理面進行粗面化及/或親水化,其次,進行將促進對被處理面上之鍍敷觸媒的吸附之吸附物質供給於被處理面上之感受性化處理(sensitization)、與於被處理面上使鍍敷觸媒吸附之活性化處理(activation)。通常情況下,感受性化處
理係浸漬被處理物於氯化亞錫之酸性溶液中,藉此,可作為還原劑作用之金屬(Sn2+)附著於被處理面。而且對於被感受性化之被處理面,作為活性化處理係浸漬被處理物於氯化鈀之酸性溶液中。藉此,溶液中之鈀離子藉由還原劑即金屬(錫離子:Sn2+)還原,作為活性鈀觸媒核附著於被處理面。如此之前處理後,浸漬於無電解鍍敷液,將金屬鍍敷膜形成於被處理面上。
如此相對於在以往之無電解鍍敷技術有必須活性化鍍敷觸媒者,報告有藉由將含有具有銨基之超枝化聚合物及Pd微粒子之組成物作為觸媒使用,未經過塗佈後活性化步驟僅直接對無電解鍍敷液浸漬,而形成無電解鍍敷之例(專利文獻1)。
[專利文獻1]國際公開第2012/141215號小冊
如上述,在以往之無電解鍍敷處理,於前處理步驟實施之粗面化處理使用有鉻化合物(鉻酸),又前處理之步驟數非常多等,正尋求環境面或成本面、煩雜操作性等之各種的改善。
進而,近年來樹脂機殼的成形技術提昇,正尋求可直
接將漂亮之殼體表面鍍敷化之方法,尤其是伴隨電子電路形成的微細化及電信號的高速化,而尋求對平滑基板的密著性高之無電解鍍敷的方法。
因此本發明專注於如此之課題,以提供一種注重環境,以少數步驟數可簡便處理,且得到充分基板密著性,作為無電解鍍敷之前處理步驟使用之新穎無電解鍍敷底塗劑作為目的。
本發明者們為了達成上述目的經努力研究的結果,發現組合於分子末端具有銨基之超枝化聚合物、金屬微粒子、具有(甲基)丙烯醯基之聚合性化合物、及光聚合起始劑,並將此塗佈於基材上所得之層作為無電解金屬鍍敷之底塗層,鍍敷性以及密著性優異,而完成本發明。
亦即,本發明作為第1觀點,係關於一種光硬化性底塗劑,其係於基材上藉由無電解鍍敷處理,用以形成金屬鍍敷膜之底塗劑,(a)於分子末端具有銨基且重量平均分子量為1,000~5,000,000之超枝化聚合物、(b)金屬微粒子、(c)具有(甲基)丙烯醯基之聚合性化合物、及(d)光聚合起始劑。
作為第2觀點,係關於第1觀點之光硬化性底塗劑,其中,前述(c)聚合性化合物係具有(甲基)丙烯醯基,且為
具有選自由氧伸烷基構造、胺基甲酸乙酯構造及聚(甲基)丙烯酸構造所構成之群組中之至少一個構造的化合物。
作為第3觀點,係關於第1觀點之光硬化性底塗劑,其中,前述(c)聚合性化合物係具有(甲基)丙烯醯基,且為具有選自由氧伸烷基構造及胺基甲酸乙酯構造所構成之群組中之至少一個構造的化合物。
作為第4觀點,係關於第2觀點之光硬化性底塗劑,其中,前述(c)聚合性化合物係具有(甲基)丙烯醯基,且為具有氧伸烷基構造的化合物。
作為第5觀點,係關於第2觀點之光硬化性底塗劑,其中,前述(c)聚合性化合物為胺基甲酸乙酯(甲基)丙烯酸酯化合物。
作為第6觀點,係關於第2觀點之光硬化性底塗劑,其中,前述(c)聚合性化合物為具有(甲基)丙烯醯基之聚(甲基)丙烯酸化合物。
作為第7觀點,係關於第1觀點~第6觀點中任一項之光硬化性底塗劑,其中,前述(c)聚合性化合物係於分子內具有2個以上(甲基)丙烯醯基之化合物。
作為第8觀點,係關於第1觀點~第7觀點中任一項之光硬化性底塗劑,其中,前述(a)超枝化聚合物為式[1]表示之超枝化聚合物。
作為第9觀點,係關於第8觀點之光硬化性底塗劑,其中,前述(a)超枝化聚合物為式[3]表示之超枝化聚合物。
作為第10觀點,係關於第1觀點~第9觀點中任一項之光硬化性底塗劑,其中,前述(b)金屬微粒子係選自由鐵(Fe)、鈷(Co)、鎳(Ni)、銅(Cu)、鈀(Pd)、銀(Ag)、錫(Sn)、鉑(Pt)及金(Au)所構成之群組中之至少一種金屬的微粒子。
作為第11觀點,係關於第10觀點之光硬化性底塗劑,其中,前述(b)金屬微粒子為鈀微粒子。
作為第12觀點,係關於第1觀點~第11觀點中任一項之光硬化性底塗劑,其中,前述(b)金屬微粒子為具有1~100nm之平均粒徑的微粒子。
作為第13觀點,係關於一種無電解鍍敷底塗層,其係將如第1觀點~第12觀點中任一項之光硬化性底塗劑藉由光硬化進行層形成而得到。
作為第14觀點,係關於一種金屬鍍敷膜,其係藉由於如第13觀點之無電解鍍敷底塗層進行無電解鍍敷,而形成於該底塗層上。
作為第15觀點,係關於一種金屬被膜基材,其係具備基材、與形成於該基材上之如第13觀點之無電解鍍敷底塗層、與形成於該無電解鍍敷底塗層上之如第14觀點之金屬鍍敷膜。
作為第16觀點,係關於一種金屬被膜基材的製造方法,其係包含下述A步驟~C步驟。
A步驟:將如第1觀點~第12觀點中任一項之光硬化性底塗劑塗佈於基材上,形成塗膜之步驟、
B步驟:將塗佈了光硬化性底塗劑之基材曝光,形成底塗層之步驟、
C步驟:將具備底塗層之基材浸漬於無電解鍍敷浴,形成金屬鍍敷膜之步驟。
本發明之底塗劑僅塗佈於基材上進行光硬化,可輕易形成無電解金屬鍍敷之底塗層。又,本發明之底塗劑,即使未形成以往為了提高與金屬鍍敷膜的密著性而形成於基材上之底漆層,亦可形成與基材的密著性優異之底塗層。進而,本發明之底塗劑可描繪μm級之細線,亦可適合使用在各種配線技術。
又由本發明之底塗劑所形成之無電解金屬鍍敷的底塗
層,僅浸漬於無電解鍍敷浴,即可輕易形成金屬鍍敷膜,可輕易得到具備基材與底塗層、以及金屬鍍敷膜的金屬被膜基材。而且上述金屬鍍敷膜係與下層之底塗層的密著性優異。
亦即,藉由使用本發明之底塗劑於基材上形成底塗層,亦即可形成與基材的密著性優異之金屬鍍敷膜。
[圖1]圖1係表示於製造例1所得之於分子末端具有氯原子的超枝化聚合物(HPS-Cl)之1H NMR光譜之圖。
[圖2]圖2係表示於製造例2所得之於分子末端具有二甲基辛基銨基的超枝化聚合物(HPS-N(Me)2OctCl)之13C NMR光譜之圖。
以下,針對本發明進行詳細說明。
本發明之底塗劑係包含(a)於分子末端具有銨基且重量平均分子量為1,000~5,000,000之超枝化聚合物、(b)金屬微粒子、(c)具有(甲基)丙烯醯基之聚合性化合物、及(d)光聚合起始劑之光硬化性底塗劑。
本發明之底塗劑係適合作為於基材上藉由無電解鍍敷處理,用以形成金屬鍍敷膜之底塗劑使用。
本發明之底塗劑所使用之超枝化聚合物係於分子末端具有銨基且重量平均分子量為1,000~5,000,000之聚合物,具體而言,可列舉下述式[1]表示之超枝化聚合物。
又,R2~R4分別獨立表示氫原子、碳原子數1~20之直鏈狀、分支狀或環狀之烷基、碳原子數7~20之芳烷基、或-(CH2CH2O)mR5(式中,R5表示氫原子或甲基,m表示2~100之任意整數)。上述烷基及芳烷基可被烷氧基、羥基、銨基、羧基或氰基取代。又,R2~R4當中之2個基一起表示直鏈狀、分支狀或環狀之伸烷基、或R2~R4可與該等鍵結之氮原子一起形成環。
又X-表示陰離子,n為重複單位構造之數,且表示5~100,000之整數。
作為在上述R2~R4之碳原子數1~20之直鏈狀烷基,可列舉甲基、乙基、n-丙基、n-丁基、n-戊基、
n-己基、n-庚基、n-辛基、n-壬基、n-癸基、n-十一烷基、n-十二烷基、n-十三烷基、n-十四烷基、n-十五烷基、n-十六烷基、n-十七烷基、n-十八烷基、n-十九烷基、n-二十烷基等,底塗劑以難以溶出於無電解鍍敷液的點來看,較佳為碳原子數8以上之基,特佳為n-辛基。作為分支狀之烷基,可列舉異丙基、異丁基、sec-丁基、tert-丁基等。作為環狀之烷基,可列舉具有環戊環、環己環構造之基等。
又,作為在R2~R4之碳原子數7~20之芳烷基,可列舉苄基、苯乙基等。
進而,作為R2~R4當中之2個基成為一起之直鏈狀之伸烷基,可列舉亞甲基、伸乙基、三亞甲基、四亞甲基、六亞甲基等。作為分支狀之伸烷基,可列舉甲基伸乙基、丁烷-1,3-二基、2-甲基丙烷-1,3-二基等。作為環狀之伸烷基,可列舉碳原子數3~30之單環式、多環式、交聯環式之環狀構造的脂環式脂肪族基。具體而言,可列舉具有碳原子數4以上之單環、雙環、三環、四環、五環構造等之基。此等伸烷基可於基中包含氮原子、硫原子或氧原子。
而且,於式[1]表示之構造,R2~R4係與該等鍵結之氮原子一起形成之環,可於環中包含氮原子、硫原子或氧原子,例如可列舉吡啶環、嘧啶環、吡嗪環、喹啉環、聯吡啶環等。
作為此等R2~R4的組合,例如可列舉[甲基、甲基、
甲基]、[甲基、甲基、乙基]、[甲基、甲基、n-丁基]、[甲基、甲基、n-己基]、[甲基、甲基、n-辛基]、[甲基、甲基、n-癸基]、[甲基、甲基、n-十二烷基]、[甲基、甲基、n-十四烷基]、[甲基、甲基、n-十六烷基]、[甲基、甲基、n-十八烷基]、[乙基、乙基、乙基]、[n-丁基、n-丁基、n-丁基]、[n-己基、n-己基、n-己基]、[n-辛基、n-辛基、n-辛基]等,其中較佳為[甲基、甲基、n-辛基]、[n-辛基、n-辛基、n-辛基]的組合。
又,作為X-之陰離子,較佳為可列舉鹵素原子、PF6 -、BF4 -或全氟烷磺酸酯。
上述式[1]中,A1表示下述式[2]表示之構造。
上述式[2]中,A2係表示可包含醚鍵或酯鍵之碳原子數1~30之直鏈狀、分支狀或環狀之伸烷基。
Y1~Y4分別獨立表示氫原子、碳原子數1~20之烷基、碳原子數1~20之烷氧基、硝基、羥基、胺基、羧基或氰基。
作為上述A2之伸烷基的具體例,可列舉亞甲基、伸乙基、三亞甲基、四亞甲基、六亞甲基等之直鏈狀伸烷基、甲基伸乙基、丁烷-1,3-二基、2-甲基丙烷-1,3-二
基等之分支狀伸烷基。又作為環狀伸烷基,可列舉碳原子數3~30之單環式、多環式及交聯環式之環狀構造的脂環式脂肪族基。具體而言,可列舉碳原子數4以上之具有單環、雙環、三環、四環、五環構造等之基。例如,於下述,脂環式脂肪族基當中,表示脂環式部分之構造例(a)~(s)。
又作為上述式[2]中Y1~Y4之碳原子數1~20之烷基,可列舉甲基、乙基、異丙基、n-戊基、環己基等。作為碳原子數1~20之烷氧基,可列舉甲氧基、乙氧基、異丙氧基、n-戊氧基、環己氧基等。作為Y1~Y4,較佳為氫原子或碳原子數1~20之烷基。
較佳為作為本發明所使用之超枝化聚合物,可列舉下述式[3]表示之超枝化聚合物。
前述式[3]中,R1~R4及n係表示與上述相同意義。
本發明所用之於分子末端具有上述銨基的超枝化聚合物,例如可藉由於分子末端具有鹵素原子的超枝化聚合物與胺化合物進行反應而得到。
尚,於分子末端具有鹵素原子的超枝化聚合物,依國際公開第2008/029688號小冊之記載,可藉由於分子末端具有二硫代胺基甲酸酯基的超枝化聚合物製造。該於分子末端具有二硫代胺基甲酸酯基的超枝化聚合物,可使用市售品,可適合使用日產化學工業(股)製之Hyper Tech(註冊商標)HPS-200等。
可於本反應使用之胺化合物,作為第一級胺,可列舉甲基胺、乙基胺、n-丙基胺、異丙基胺、n-丁基胺、異丁基胺、sec-丁基胺、tert-丁基胺、n-戊基胺、n-己基胺、n-庚基胺、n-辛基胺、n-壬基胺、n-癸基胺、n-十一烷基胺、n-十二烷基胺、n-十三烷基胺、n-十四烷基胺、n-十五烷基胺、n-十六烷基胺、n-十七烷基胺、n-十八烷基胺、n-十九烷基胺、n-二十烷基胺等之脂肪族胺;環戊基胺、環己基胺等之脂環式胺;苄基胺、苯乙基胺等之芳烷基胺;苯胺、p-n-丁基苯胺、p-tert-丁基苯胺、p-n-辛基苯胺、p-n-癸基苯胺、p-n-十二烷基苯胺、p-n-十四烷基苯胺等之苯胺類、1-萘基胺、2-萘基胺等之萘基胺類、1-胺蒽(Aminoanthracene)、2-胺蒽等之胺蒽類、1-胺基蒽醌等之胺基蒽醌類、4-胺基聯苯、2-胺基聯苯等之胺基聯苯類、2-胺基茀、1-胺基-9-芴酮、4-胺基-9-芴酮等之胺基茀類、5-胺基茚烷等之胺基茚烷類、5-胺基異喹啉等之胺基異喹啉類、9-胺基菲等之胺基菲類等之芳香族胺。進而可列舉N-(tert-丁氧基羰基)-1,2-乙二胺(Ethylenediamine)、N-(tert-丁氧基羰基)-1,3-丙二胺、N-(tert-丁氧基羰基)-1,4-丁二胺、N-(tert-丁氧基羰基)-1,5-五亞甲基二胺、N-(tert-丁氧基羰基)-1,6-六亞甲基二胺、N-(2-羥基乙基)胺、N-(3-羥基丙基)胺、N-(2-甲氧基乙基)胺、N-(2-乙氧基乙基)胺等之胺化合物。
作為第二級胺,可列舉二甲基胺、二乙基胺、二-n-丙基胺、二異丙基胺、二-n-丁基胺、二異丁基
胺、二-sec-丁基胺、二-n-戊基胺、乙基甲基胺、甲基-n-丙基胺、甲基-n-丁基胺、甲基-n-戊基胺、乙基異丙基胺、乙基-n-丁基胺、乙基-n-戊基胺、甲基-n-辛基胺、甲基-n-癸基胺、甲基-n-十二烷基胺、甲基-n-十四烷基胺、甲基-n-十六烷基胺、甲基-n-十八烷基胺、乙基異丙基胺、乙基-n-辛基胺、二-n-己基胺、二-n-辛基胺、二-n-十二烷基胺、二-n-十六烷基胺、二-n-十八烷基胺等之脂肪族胺;二環己基胺等之脂環式胺;二苄基胺等之芳烷基胺;二苯基胺等之芳香族胺;苯二甲醯亞胺、吡咯、哌啶、哌嗪、咪唑等之含氮之雜環式化合物。進而可列舉雙(2-羥基乙基)胺、雙(3-羥基丙基)胺、雙(2-乙氧基乙基)胺、雙(2-丙氧基乙基)胺等。
作為第三級胺,可列舉三甲基胺、三乙基胺、三-n-丙基胺、三-n-丁基胺、三-n-戊基胺、三-n-己基胺、三-n-辛基胺、三-n-十二烷基胺、二甲基乙基胺、二甲基-n-丁基胺、二甲基-n-己基胺、二甲基-n-辛基胺、二甲基-n-癸基胺、二乙基-n-癸基胺、二甲基-n-十二烷基胺、二甲基-n-十四烷基胺、二甲基-n-十六烷基胺、二甲基-n-十八烷基胺、二甲基-n-二十烷基胺等之脂肪族胺;吡啶、吡嗪、嘧啶、喹啉、1-甲基咪唑、4,4’-聯吡啶、4-甲基-4,4’-聯吡啶等含氮之雜環式化合物。
可於此等之反應使用之胺化合物的使用量,相對於於分子末端具有鹵素原子的超枝化聚合物之鹵素原子1莫耳,可為0.1~20莫耳當量,較佳可為0.5~10莫
耳當量,更佳可為1~5莫耳當量。
於分子末端具有鹵素原子的超枝化聚合物與胺化合物的反應,可於水或有機溶劑中,於鹼的存在下或非存在下進行。使用之溶劑,較佳為可溶解於分子末端具有鹵素原子的超枝化聚合物與胺化合物者。進而,若為雖可溶解於分子末端具有鹵素原子的超枝化聚合物與胺化合物,但無法溶解於分子末端具有銨基的超枝化聚合物之溶劑,單離變容易而更適合。
作為可於本反應使用之溶劑,若為不會顯著阻礙本反應進行者即可,可使用水;2-丙醇等之醇類;乙酸等之有機酸類;苯、甲苯、二甲苯、乙基苯、1,2-二氯苯等之芳香族烴類;四氫呋喃(THF)、二乙醚等之醚類;丙酮、甲基乙基酮(MEK)、甲基異丁基酮(MIBK)、環己酮等之酮類;氯仿、二氯甲烷、1,2-二氯乙烷等之鹵素化物;n-己烷、n-庚烷、環己烷等之脂肪族烴類;N,N-二甲基甲醯胺(DMF)、N,N-二甲基乙醯胺、N-甲基-2-吡咯烷酮(NMP)等之醯胺類。此等之溶劑可使用1種,亦可混合2種以上使用。又,使用量相對於於分子末端具有鹵素原子的超枝化聚合物的質量,以使用0.2~1,000倍質量,較佳為1~500倍質量,更佳為5~100倍質量,最佳為5~50倍質量的溶劑較佳。
作為適合的鹼,一般而言係使用鹼金屬氫氧化物及鹼土類金屬氫氧化物(例如氫氧化鈉、氫氧化鉀、氫氧化鈣)、鹼金屬氧化物及鹼土類金屬氧化物(例如氧化
鋰、氧化鈣)、鹼金屬氫化物及鹼土類金屬氫化物(例如氫化鈉、氫化鉀、氫化鈣)、鹼金屬醯胺(例如鈉醯胺)、鹼金屬碳酸鹽及鹼土類金屬碳酸鹽(例如碳酸鋰、碳酸鈉、碳酸鉀、碳酸鈣)、鹼金屬重碳酸鹽(例如重碳酸鈉)等之無機化合物、以及鹼金屬烷基、烷基鎂鹵素化物、鹼金屬烷氧化物、鹼土類金屬烷氧化物、二甲氧基鎂等之有機金屬化合物。特佳為碳酸鉀及碳酸鈉。又,使用量相對於於分子末端具有鹵素原子的超枝化聚合物之鹵素原子1莫耳,以使用0.2~10莫耳當量,較佳為0.5~10莫耳當量,最佳為1~5莫耳當量的鹼較佳。
於此反應,較佳為於反應開始前充分去除反應系內的氧,以氮、氬等之惰性氣體取代系統內即可。作為反應條件。反應時間從0.01~100小時、反應溫度從0~300℃適當選擇。較佳係反應時間為0.1~72小時,反應溫度為20~150℃。
使用第三級胺時,不管鹼的存在/非存在,都可得到式[1]表示之超枝化聚合物。
於鹼的非存在下,使第一級胺或第二級胺化合物與於分子末端具有鹵素原子的超枝化聚合物進行反應時,得到分別對應之超枝化聚合物的末端第二級胺及第三級胺經質子化之銨基末端的超枝化聚合物。又,即使在使用鹼進行反應時,藉由於有機溶劑中與氯化氫、溴化氫、碘化氫等之酸的水溶液混合,得到對應之超枝化聚合物的末端第二級胺及第三級胺經質子化之銨基末端的超枝化聚合物。
前述超枝化聚合物藉由凝膠滲透層析以聚苯乙烯換算所測定之重量平均分子量Mw為1,000~5,000,000,更佳為2,000~200,000,最佳為3,000~100,000。又,作為分散度Mw(重量平均分子量)/Mn(數平均分子量)為1.0~7.0,較佳為1.1~6.0,更佳為1.2~5.0。
作為本發明之底塗劑所使用之金屬微粒子,並未特別限定,作為金屬種,可列舉鐵(Fe)、鈷(Co)、鎳(Ni)、銅(Cu)、鈀(Pd)、銀(Ag)、錫(Sn)、鉑(Pt)及金(Au)以及此等之合金,可此等之金屬之1種,亦可為2種以上之併用亦無妨。其中作為較佳之金屬微粒子,可列舉鈀微粒子。尚,作為金屬微粒子,亦可使用前述金屬之氧化物。
前述金屬微粒子,例如由金屬鹽之水溶液藉由高壓水銀燈進行光照射之方法、或於該水溶液添加具有還原作用之化合物(所謂還原劑)之方法等,藉由還原金屬離子而得到。例如,添加金屬鹽之水溶液於溶解上述超枝化聚合物之溶液,並對此照射紫外線、或於該超枝化聚合物溶液添加金屬鹽之水溶液及還原劑等,藉由還原金屬離子,可形成超枝化聚合物與金屬微粒子的複合體,同時可調製包含超枝化聚合物及金屬微粒子之底塗劑。
作為前述金屬鹽,可列舉氯化金酸、硝酸銀、硫酸銅、硝酸銅、乙酸銅、氯化錫、氯化鉑、氯化鉑
酸、Pt(dba)2[dba=二苯亞基丙酮]、Pt(cod)2[cod=1,5-環辛二烯]、Pt(CH3)2(cod)、氯化鈀、乙酸鈀(Pd(OC(=O)CH3)2)、硝酸鈀、Pd2(dba)3.CHCl3、Pd(dba)2、氯化銠、乙酸銠、氯化釕、乙酸釕、Ru(cod)(cot)[cot=環辛三烯]、氯化銥、乙酸銥、Ni(cod)2等。
作為前述還原劑,並非被特別限定者,可使用各種還原劑,以依照所得之底塗劑所含有之金屬種等來選擇還原劑較佳。作為可使用之還原劑,例如可列舉氫化硼鈉、氫化硼鉀等之氫化硼金屬鹽;氫化鋁鋰、氫化鋁鉀、氫化鋁銫、氫化鋁鈹、氫化鋁鎂、氫化鋁鈣等之氫化鋁鹽;肼化合物;檸檬酸及其鹽;琥珀酸及其鹽;抗壞血酸及其鹽;甲醇、乙醇、2-丙醇、多元醇等之第一級或第二級醇類;三甲基胺、三乙基胺、二異丙基乙基胺、二乙基甲基胺、四甲基乙二胺(TMEDA)、乙二胺四乙酸(EDTA)等之第三級胺類;羥基胺;三-n-丙基膦、三-n-丁基膦、三環己基膦、三苄基膦、三苯基膦、三乙氧基膦、1,2-雙(二苯基膦基)乙烷(DPPE)、1,3-雙(二苯基膦基)丙烷(DPPP)、1,1’-雙(二苯基膦基)二茂鐵(DPPF)、2,2’-雙(二苯基膦基)-1,1’-聯萘基(BINAP)等之膦類等。
前述金屬微粒子之平均粒徑較佳為1~100nm。藉由將該金屬微粒子之平均粒徑定為100nm以下,表面積的減少變少且得到充分之觸媒活性。作為平均粒徑,更佳為75nm以下,特佳為1~30nm。
在本發明之底塗劑之上述(a)超枝化聚合物的添加量,相對於上述(b)金屬微粒子100質量份,較佳為50~2,000質量份。藉由成為50質量份以上,可充分分散上述金屬微粒子,又藉由成為2,000質量份以下,可抑制起因於有機物含量增加之物性等之問題。更佳為100~1,000質量份。
作為本發明之底塗劑所使用之具有(甲基)丙烯醯基之聚合性化合物,較佳為具有(甲基)丙烯醯基,且具有選自由氧伸烷基構造、胺基甲酸乙酯構造及聚(甲基)丙烯酸構造所構成之群組中之至少一個構造的化合物,或較佳為具有(甲基)丙烯醯基,且具有選自由氧伸烷基構造及胺基甲酸乙酯構造所構成之群組中之至少一個構造的化合物。特佳為具有(甲基)丙烯醯基且具有氧伸烷基構造的化合物、胺基甲酸乙酯(甲基)丙烯酸酯化合物、或具有(甲基)丙烯醯基之聚(甲基)丙烯酸化合物。又,具有(甲基)丙烯醯基之聚合性化合物,較佳為於分子內具有2個以上(甲基)丙烯醯基。
作為上述氧伸烷基構造,例如可列舉具有氧伸烷基之構造,作為上述氧伸烷基,較佳為碳原子數2~4之氧伸烷基,其中較佳為氧乙烯基[-OCH2CH2-]或氧丙烯基[-OCH2C(CH3)H-]。氧伸烷基可為複數個連結之聚(氧伸烷)基,該情況下,可單獨具有一種氧伸烷基、或是組合
二種以上而具有。具有複數種之氧伸烷基時,該等之結合可為嵌段結合及無規結合之任一種。
尚,於本發明所謂(甲基)丙烯酸酯化合物,係指丙烯酸酯化合物與甲基丙烯酸酯化合物雙方。例如(甲基)丙烯酸係指丙烯酸與甲基丙烯酸。
作為如此之化合物,例如例示以下之(1)~(5)所示之有機化合物。
作為具有1個(甲基)丙烯醯基且具有氧伸烷基構造的化合物,例如可列舉2-苯氧基乙基(甲基)丙烯酸酯、氧化乙烯改質o-苯基酚(甲基)丙烯酸酯、乙二醇單甲醚(甲基)丙烯酸酯、乙二醇單乙醚(甲基)丙烯酸酯、二乙二醇單(甲基)丙烯酸酯、二乙二醇單甲醚(甲基)丙烯酸酯、二乙二醇單乙醚(甲基)丙烯酸酯、二乙二醇單丁醚(甲基)丙烯酸酯、二乙二醇單(2-乙基己基)醚(甲基)丙烯酸酯、二乙二醇單苯醚(甲基)丙烯酸酯、三乙二醇單甲醚(甲基)丙烯酸酯、四乙二醇單甲醚(甲基)丙烯酸酯、四乙二醇單月桂醚(甲基)丙烯酸酯、四乙二醇單(壬基苯基)醚(甲基)丙烯酸酯、八乙二醇單(甲基)丙烯酸酯、九乙二醇單甲醚(甲基)丙烯酸酯、十乙二醇單(甲基)丙烯酸酯、十三乙二醇單甲醚(甲基)丙烯酸酯、聚乙二醇單(甲基)丙烯酸酯、聚乙二
醇單甲醚(甲基)丙烯酸酯、二丙二醇單甲醚(甲基)丙烯酸酯、三丙二醇單(甲基)丙烯酸酯、四丙二醇單(甲基)丙烯酸酯、五丙二醇單(壬基苯基)醚(甲基)丙烯酸酯、六丙二醇單(甲基)丙烯酸酯、九丙二醇單(甲基)丙烯酸酯、十三丙二醇單(甲基)丙烯酸酯、聚丙二醇單(甲基)丙烯酸酯、聚丙二醇單甲醚(甲基)丙烯酸酯等。
上述單官能化合物可適合使用市售品,例如可列舉2-MTA、MPE400A、MPE550A、Viscoat#192、同#192D、同#190、同#MTG[以上皆為大阪有機化學工業(股)製];Light Acrylate EC-A、同MTG-A、同EHDG-AT、同130A、同DPM-A、同PO-A、同P2H-A、同P-200A、同NP-4EA、Light EsterBC、同130MA、同041MA、同PO[以上皆為共榮社化學(股)製];NK ester A-LEN-10、同AM-90G、同AM-130G、同AMP-20GY、同M-90G、同M-230G、同PHE-1G[以上皆為新中村化學工業(股)製];EBECRYL(註冊商標)110、同114[以上皆為DAICEL-ALLNEX(股)製];BLEMMER(註冊商標)AE-90U、同AE-200、同AE-400、同AP-150、同AP-400、同AP-550、同AP-800、同AME-400、同ALE-200、同ANP-300、同75ANEP-600、同AAE-300、同PE-90、同PE-200、同PE-350、同PE-350G、同PP-1000、同PP-500、同PP-800、同50PEP-300、同70PEP-350B、同55PET-800、同10PPB-500B、同PME-100、同PME-200、同PME-400、同PME-1000、同PME-4000、同50POEP-
800B、同PLE-200、同PLE-1300、同PSE-1300、同PAE-100、同43PAPE-600B[以上皆為日油(股)製]等。
作為具有2個(甲基)丙烯醯基且具有氧伸烷基構造的化合物,例如可列舉二乙二醇二(甲基)丙烯酸酯、三乙二醇二(甲基)丙烯酸酯、四乙二醇二(甲基)丙烯酸酯、七乙二醇二(甲基)丙烯酸酯、九乙二醇二(甲基)丙烯酸酯、十四乙二醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、二丙二醇二(甲基)丙烯酸酯、三丙二醇二(甲基)丙烯酸酯、七丙二醇二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯、三(四亞甲基甘醇)二(甲基)丙烯酸酯、九(四亞甲基甘醇)二(甲基)丙烯酸酯、聚(四亞甲基甘醇)二(甲基)丙烯酸酯、氧化丙烯改質新戊二醇二(甲基)丙烯酸酯、氧化乙烯改質雙酚A二(甲基)丙烯酸酯[氧化乙烯加成莫耳數2~30]、氧化丙烯改質雙酚A二(甲基)丙烯酸酯[氧化丙烯加成莫耳數2~30]、氧化乙烯-氧化丙烯改質雙酚A二(甲基)丙烯酸酯、9,9-雙(4-(2-((甲基)丙烯醯氧基)乙氧基)苯基)茀等。
上述2官能化合物可適合使用市售品,例如可列舉Viscoat#310HP、同#335HP、同#700HV[以上皆為大阪有機化學工業(股)製];Light Acrylate 3EG-A、同4EG-A、同9EG-A、同14EG-A、同PTMGA-250、同BP-4EAL、同BP-4PA、Light Ester2EG、同3EG、同4EG、
同9EG、同14EG、同BP-2EMK[以上皆為共榮社化學(股)製];NK ester A-200、同A-400、同A-600、同A-B1206PE、同ABE-300、同A-BPE-4、同A-BPE-10、同A-BPE-20、同A-BPE-30、同A-BPEF、同A-BPP-3、同APG-100、同APG-200、同APG-400、同APG-700、同A-PTMG-65、同2G、同3G、同4G、同9G、同14G、同23G、同BPE-80N、同BPE-100、同BPE-200、同BPE-500、同BPE-900、同BPE-1300N、同1206PE、同9PG[以上皆為新中村化學工業(股)製];DPGDA、TPGDA、PEG400DA-D、EBECRYL(註冊商標)145、同150、同11[以上皆為DAICEL-ALLNEX(股)製];BLEMMER(註冊商標)ADE-200、同ADE-300、同ADE-400、同ADE-600、同ADP-400、同ADT-250、同ADC系列、同PDE-100、同PDE-150、同PDE-200、同PDE-400、同PDE-600、同PDP-400N、同PDT-650、同PDC系列、同PDBE-200、同PDBE-250、同PDBE-450、同PDBE-1300、同PDBPE系列[以上皆為日油(股)製]等。
作為具有3個(甲基)丙烯醯基且具有氧伸烷基構造的化合物,例如可列舉氧化乙烯改質1,1,1-三羥甲基乙烷三(甲基)丙烯酸酯[氧化乙烯加成莫耳數3~30]、氧化乙烯改質三羥甲基丙烷三(甲基)丙烯酸酯[氧化乙烯加成莫耳數3~30]、氧化丙烯改質三羥甲基丙烷三(甲基)丙烯酸酯[氧
化丙烯加成莫耳數3~30]、氧化乙烯改質甘油三(甲基)丙烯酸酯[氧化乙烯加成莫耳數3~30]、氧化丙烯改質甘油三(甲基)丙烯酸酯[氧化丙烯加成莫耳數3~30]、參(2-(丙烯醯氧基)乙基)異氰脲酸酯、ε-己內酯改質參(2-(丙烯醯氧基)乙基)異氰脲酸酯[ε-己內酯加成莫耳數1~30]等。
上述3官能化合物可適合使用市售品,例如可列舉Viscoat#360[大阪有機化學工業(股)製];NK ester A-GLY-9E、同A-GLY-20E、同AT-20E[以上皆為新中村化學工業(股)製];TMPEOTA、OTA480、EBECRYL(註冊商標)135[以上皆為DAICEL-ALLNEX(股)製]等。
作為具有4個(甲基)丙烯醯基且具有氧伸烷基構造的化合物,例如可列舉氧化乙烯改質二三羥甲基丙烷四(甲基)丙烯酸酯[氧化乙烯加成莫耳數4~40]、氧化乙烯改質季戊四醇四(甲基)丙烯酸酯[氧化乙烯加成莫耳數4~40]等。
上述4官能化合物可適合使用市售品,例如可列舉NK ester ATM-4E、同ATM-35E[以上皆為新中村化學工業(股)製];EBECRYL(註冊商標)40[DAICEL-ALLNEX(股)製]等。
作為具有5個以上(甲基)丙烯醯基且具有氧伸烷基構
造的化合物,例如可列舉氧化乙烯改質二季戊四醇六(甲基)丙烯酸酯[氧化乙烯加成莫耳數6~60]、氧化乙烯改質三季戊四醇八(甲基)丙烯酸酯[氧化乙烯加成莫耳數6~60]等。
上述5官能以上之化合物可適合使用市售品,例如可列舉NK ester A-DPH-12E[新中村化學工業(股)製]等。
作為如此之化合物,例如例示以下之(1)~(6)所示之有機化合物。
作為具有1個(甲基)丙烯醯基且具有胺基甲酸乙酯構造的化合物,雖並未特別限定,但例如使聚異氰酸酯(異氰酸酯成分)與一元醇(活性氫成分)進行反應,而得到異氰酸酯末端預聚物,將此與(甲基)丙烯醯基及具有與異氰酸酯反應性之基的化合物進行反應,可得到每一分子平均具有1個(甲基)丙烯醯基的胺基甲酸乙酯(甲基)丙烯酸酯。雖可取代一元醇改使用多元醇,但該情況係必須進行於多元醇之末端羥基的一部分不導入(甲基)丙烯醯氧基的方式之操作。
作為具有2個(甲基)丙烯醯基且具有胺基甲酸乙酯構造的化合物,例如可列舉苯基縮水甘油醚之(甲基)丙烯酸加成物與六亞甲基二異氰酸酯的胺基甲酸乙酯化物、苯基縮水甘油醚之(甲基)丙烯酸加成物與甲苯二異氰酸酯的胺基甲酸乙酯化物等。
上述2官能胺基甲酸乙酯(甲基)丙烯酸酯可適合使用市售品,例如可列舉AH-600、AT-600[以上皆為共榮社化學(股)製];NKOligoU-2PPA、同U-200PA、同UA-160TM、同UA-290TM、同UA-4200、同UA-4400、同UA-122P、同UA-W2A[以上皆為新中村化學工業(股)製];EBECRYL(註冊商標)210、同215、同230、同244、同245、同270、同280/15IB、同284、同285、同4858、同8307、同8402、同8411、同8804、同8807、同9227EA、同9270、KRM(註冊商標)7735[以上皆為DAICEL-ALLNEX(股)製];紫光(註冊商標)UV-6630B、同7000B、同7461TE、同2000B、同2750B、同3000、同3200B、同3210EA、同3300B、同3310B、同3500BA、同3520TL、同3700B、同6640B[以上皆為日本合成化學工業(股)製]等。
作為具有3個(甲基)丙烯醯基且具有胺基甲酸乙酯構造的化合物之市售品,例如可列舉NKOligoUA-7100[新中村化學工業(股)製];EBECRYL(註冊商標)204、同205、同264、同265、同294/25HD、同1259、同4820、同8311、同8465、同8701、同9260、KRM(註冊商標)8296、同8667[以上皆為DAICEL-ALLNEX(股)製];紫光(註冊商標)UV-7550B、同7000B、同7510B、同7461TE、同2750B[以上皆為日本合成化學工業(股)製]等。
作為具有4個(甲基)丙烯醯基且具有胺基甲酸乙酯構造的化合物之市售品,例如可列舉EBECRYL(註冊商標)8210、同8405、KRM(註冊商標)8528[以上皆為DAICEL-ALLNEX(股)製];紫光(註冊商標)UV-7650B[日本合成化學工業(股)製]等。
作為具有5個以上(甲基)丙烯醯基且具有胺基甲酸乙酯構造的化合物,例如可列舉季戊四醇三(甲基)丙烯酸酯與六亞甲基二異氰酸酯的胺基甲酸乙酯化物、季戊四醇三(甲基)丙烯酸酯與甲苯二異氰酸酯的胺基甲酸乙酯化物、
季戊四醇三(甲基)丙烯酸酯與異佛爾酮二異氰酸酯的胺基甲酸乙酯化物、二季戊四醇五(甲基)丙烯酸酯與六亞甲基二異氰酸酯的胺基甲酸乙酯化物等。
上述5官能以上之胺基甲酸乙酯(甲基)丙烯酸酯可適合使用市售品,例如可列舉UA-306H、UA-306T、UA-306I、UA-510H[以上皆為共榮社化學(股)製];NKOligo U-6LPA、同U-10HA、同U-10PA、同U-1100H、同U-15HA、同UA-53H、同UA-33H[以上皆為新中村化學工業(股)製];EBECRYL(註冊商標)220、同1290、同5129、同8254、同8301R、KRM(註冊商標)8200、同8200AE、同8904、同8452[以上皆為DAICEL-ALLNEX(股)製];紫光(註冊商標)UV-1700B、同6300B、同7600B、同7605B、同7610B、同7620EA、同7630B、同7640B、同7650B[以上皆為日本合成化學工業(股)製]等。
聚胺基甲酸乙酯(甲基)丙烯酸酯可適合使用市售品,例如可列舉ACRIT8BR-500、同8BR-600、同8BR-930M[以上皆為大成Fine chemical(股)製]等之於側鏈具有胺基甲酸乙酯構造的聚胺基甲酸乙酯(甲基)丙烯酸酯;ACRIT8UH-1006、同8UH-1012[以上皆為大成Fine chemical(股)製]等之於主鏈具有胺基甲酸乙酯構造的聚胺基甲酸乙酯(甲基)丙烯酸酯等。
作為如此之化合物,若為於側鏈具有(甲基)丙烯醯基之(甲基)丙烯酸聚合物,並未特別限制。如此之聚合物(亦稱為(甲基)丙烯酸(甲基)丙烯酸酯),例如可藉由聚合(甲基)丙烯酸單體,其係將具有反應性基之(甲基)丙烯酸酯作為單體成分包含,於所得之聚合物,使具有可與該反應性基反應之官能基與(甲基)丙烯醯基的化合物進行反應而得到。
上述(甲基)丙烯酸(甲基)丙烯酸酯可適合使用市售品,例如可列舉ACRIT8KX-077、同8KX-078、同8KX-127、同8KX-128、同8KX-012C、同8KX-014C、同8KX-018C、同8KX-052C、同8KQ-2001[以上皆為大成Fine chemical(股)製];SMP-220A、SMP-250A、SMP-360A、SMP-550A[以上皆為共榮社化學(股)製]等。
又,作為本發明之底塗劑所使用之具有(甲基)丙烯醯基之聚合性化合物,除了具有上述(甲基)丙烯醯基,且具有選自由氧伸烷基構造、胺基甲酸乙酯構造及聚(甲基)丙烯酸構造所構成之群組中之至少一個構造的化合物之外,亦以於分子內具有2個以上(甲基)丙烯醯基之化合物較佳。
作為除了具有上述(甲基)丙烯醯基且具有氧伸烷基構造的化合物、上述胺基甲酸乙酯(甲基)丙烯酸酯化合物以及上述具有(甲基)丙烯醯基之聚(甲基)丙烯酸化合物之外的本發明之(c)聚合性化合物,例如例示以下(1)~(5)所示之有機化合物。
作為具有1個(甲基)丙烯醯基之化合物,例如可列舉甲基(甲基)丙烯酸酯、乙基(甲基)丙烯酸酯、丙基(甲基)丙烯酸酯、丁基(甲基)丙烯酸酯、異丁基(甲基)丙烯酸酯、tert-丁基(甲基)丙烯酸酯、異戊基(甲基)丙烯酸酯、己基(甲基)丙烯酸酯、環己基(甲基)丙烯酸酯、辛基(甲基)丙烯酸酯、異辛基(甲基)丙烯酸酯、2-乙基己基(甲基)丙烯酸酯、壬基(甲基)丙烯酸酯、異壬基(甲基)丙烯酸酯、3,5,5-三甲基己基(甲基)丙烯酸酯、癸基(甲基)丙烯酸酯、異癸基(甲基)丙烯酸酯、4-tert-丁基環己基(甲基)丙烯酸酯、金剛烷基(甲基)丙烯酸酯、降冰片烯基(甲基)丙烯酸酯、異莰基(甲基)丙烯酸酯、薄荷基(Menthyl)(甲基)丙烯酸酯、十一烷基(甲基)丙烯酸酯、月桂基(甲基)丙烯酸酯、十三烷基(甲基)丙烯酸酯、棕櫚基(甲基)丙烯酸酯、硬脂基(甲基)丙烯酸酯、異硬脂基(甲基)丙烯酸酯、二十二烷基(甲基)丙烯酸酯、苄基(甲基)丙烯酸酯、縮水甘油基(甲基)丙烯酸酯、四氫糠基(甲基)丙烯酸酯、2-羥基乙基(甲基)丙烯酸酯、2-羥基丙基(甲基)丙烯酸酯、甘
油單(甲基)丙烯酸酯、2-羥基-3-苯氧基丙基(甲基)丙烯酸酯、2-羥基丁基(甲基)丙烯酸酯、4-羥基丁基(甲基)丙烯酸酯、2-羥基乙基=(2-((甲基)丙烯醯氧基)乙基)=苯二甲酸酯、β-羧基乙基(甲基)丙烯酸酯、單(2-((甲基)丙烯醯氧基)乙基)琥珀酸酯、單(2-((甲基)丙烯醯氧基)乙基)六氫苯二甲酸酯、單(2-((甲基)丙烯醯氧基)乙基)苯二甲酸酯、新戊二醇=苯甲酸酯=(甲基)丙烯酸酯、二甲基胺基乙基(甲基)丙烯酸酯、二乙基胺基乙基(甲基)丙烯酸酯、7-胺基-3,7-二甲基辛基(甲基)丙烯酸酯、異丙基(甲基)丙烯酸醯胺、tert-辛基(甲基)丙烯酸醯胺、異丁氧基甲基(甲基)丙烯酸醯胺、二丙酮(甲基)丙烯酸醯胺、2-羥基乙基(甲基)丙烯酸醯胺、3-(N,N-二甲基胺基)丙基(甲基)丙烯酸醯胺、N,N-二甲基(甲基)丙烯酸醯胺、N,N-二乙基(甲基)丙烯酸醯胺、(甲基)丙烯醯嗎啉等。
上述單官能化合物可適合使用市售品,例如可列舉HEA、HPA、4-HBA、AIB、TBA、NOAA、IOAA、INAA、LA、STA、ISTA、IBXA、MEDOL-10、OXE-10、OXE-30、Viscoat#150、同#150D、同#155、同#160、同#190D[以上皆為大阪有機化學工業(股)製];Light EsterE、同NB、同IB、同TB、同EH、同ID、同L、同L-7、同S、同CH、同THF(1000)、同BZ、同IB-X、同HO-250(N)、同HOP(N)、同HOA(N)、同HOP-A(N)、同HOB(N)、同DM、同DE、同DQ-100、同HO-MS(N)、同HO-HH(N)、同G、同P-1M、同P-2M、Light
Acrylate IAA、同L-A、同S-A、同THF-A、同IB-XA、同HOB-A、同HOA-HH(N)、同BA-104、同P-1A(N)、環氧酯M-600A、HOA-MS(N)、HOA-MPL(N)、HOA-MPE(N)[以上皆為共榮社化學(股)製];DMAA(註冊商標)、ACMO(註冊商標)、NIPAM(註冊商標)、DEAA(註冊商標)、DMAPAA(註冊商標)、HEAA(註冊商標)[以上皆為KJChemicals(股)製];NK ester A-SA、同S-1800A、同CB-1、同S、同SA[以上皆為新中村化學工業(股)製];β-CEA、IBOA-B、ODA-N[以上皆為DAICEL-ALLNEX(股)製];BLEMMER(註冊商標)CHA、同TBCHA、同LA、同CA、同SA、同VA、同G、同GH、同GS、同GLM、同GLM-R、同G-FA80、同QA、同CHMA、同EHMA-25、同TBCHMA、同DMA、同LMA、同SLMA-S、同SLMA-SH、同CMA、同SMA、同VMA、同VMA-70[以上皆為日油(股)製]等。
作為具有2個(甲基)丙烯醯基之化合物,例如可列舉乙二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、3-甲基-1,5-戊二醇二(甲基)丙烯酸酯、1,9-壬二醇二(甲基)丙烯酸酯、1,10-癸二醇二(甲基)丙烯酸酯、2-甲基-1,8-辛二醇二(甲基)丙烯酸酯、三環[5.2.1.02,6]癸烷二甲醇二(甲基)丙烯酸酯、雙酚A二縮水甘油醚丙烯酸加成物、
羥基特戊酸新戊二醇丙烯酸加成物、甘油二(甲基)丙烯酸酯、2-羥基-3-丙烯醯氧基丙基甲基丙烯酸酯等。
上述2官能化合物可適合使用市售品,例如可列舉Viscoat#195、同#230、同#230D、同#260、同#540[以上皆為大阪有機化學工業(股)製];Light Acrylate NP-A、同MPD-A、同1.6HX-A、同1.9ND-A、同MOD-A、同DCP-A、同HPP-A、同G-201P、Light EsterP-2M、同EG、同1.4BG、同NP、同1.6HX、同1.9ND、同G-101P、同G-201P[以上皆為共榮社化學(股)製];NK ester 701A、同A-DCP、同A-DOD-N、同A-HD-N、同A-NOD-N、同1G、同DCP、同DOD-N、同HD-N、同NOD-N、同NPG、同701[以上皆為新中村化學工業(股)製];HDDA、IRR214-K、HPNDA[以上皆為DAICEL-ALLNEX(股)製];BLEMMER(註冊商標)GAM、同GAM-R、同GMR-H、同GMR-R、同NDMA[以上皆為日油(股)製]等。
作為具有3個(甲基)丙烯醯基之化合物,例如可列舉1,1,1-三羥甲基乙烷三(甲基)丙烯酸酯、三羥甲基丙烷三(甲基)丙烯酸酯、二三羥甲基丙烷三(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、甘油三(甲基)丙烯酸酯等。
上述3官能化合物可適合使用市售品,例如可列舉Viscoat#295、同#300[以上皆為大阪有機化學工業(股)製];Light Acrylate TMP-A、同PE-3A、Light
EsterTMP[以上皆為共榮社化學(股)製];NK ester A-9300、同A-9300-1CL、同A-TMM-3、同A-TMM-3L、同A-TMM-3LM-N、同A-TMPT、同TMPT[以上皆為新中村化學工業(股)製];PETIA、PETRA、TMPTA、EBECRYL(註冊商標)180[以上皆為DAICEL-ALLNEX(股)製]等。
作為具有4個(甲基)丙烯醯基之化合物,例如可列舉二三羥甲基丙烷四(甲基)丙烯酸酯、季戊四醇四(甲基)丙烯酸酯等。
上述4官能化合物可適合使用市售品,例如可列舉Viscoat#300[大阪有機化學工業(股)製];Light Acrylate PE-4A[共榮社化學(股)製];NK ester AD-TMP、同A-TMMT[以上皆為新中村化學工業(股)製];EBECRYL(註冊商標)140、同1142、同180[以上皆為DAICEL-ALLNEX(股)製]等。
作為具有5個以上(甲基)丙烯醯基之化合物,例如可列舉二季戊四醇五(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯、三季戊四醇八(甲基)丙烯酸酯等。
上述5官能以上之化合物可適合使用市售品,例如可列舉Viscoat#802[大阪有機化學工業(股)製];
Light Acrylate DPE-6A[共榮社化學(股)製];NK ester A-9550、同A-DPH[以上皆為新中村化學工業(股)製];DPHA[DAICEL-ALLNEX(股)製]等。
在本發明之底塗劑的上述(c)具有(甲基)丙烯醯基之聚合性化合物的添加量,相對於由前述超枝化聚合物與金屬微粒子所形成之複合體100質量份,較佳為0.1~500質量份,更佳為1~200質量份,再更佳為1~100質量份。
作為本發明之底塗劑所使用之光聚合起始劑,可使用周知者,例如可列舉烷基苯甲酮類、二苯甲酮類、醯基膦氧化物類、米氏之苯甲醯基苯甲酸酯類、肟酯類、四甲基單硫化甲硫碳醯胺(Thiuram Monosulfide)類、噻噸酮類等。
特佳為光開裂型之光自由基聚合起始劑。對於光開裂型之光自由基聚合起始劑,可列舉最新UV硬化技術(159頁、發行人:高薄一弘、發行所:(股)技術情報協會、1991年發行)所記載者。
作為市售之光自由基聚合起始劑,例如可列舉IRGACURE(註冊商標)184、同369、同651、同500、同819、同907、同784、同2959、同CGI1700、同CGI1750、同CGI1850、同CG24-61、同TPO、同OXE-01、同OXE-02、Darocur(註冊商標)1116、同1173[以
上、BASF日本(股)製]、ESACURE KIP150、同KIP65LT、同KIP100F、同KT37、同KT55、同KTO46、同KIP75[以上、Lamberti公司製]等。此等聚合起始劑可組合複數種使用。
光聚合起始劑可一種單獨、或混合二種以上使用。又,作為其添加量,相對於(c)聚合性化合物100質量份,為0.01~20質量份,更佳為0.1~10質量份。
本發明之底塗劑,係包含(a)於分子末端具有前述銨基的超枝化聚合物、(b)金屬微粒子、(c)聚合性化合物、及(d)光聚合起始劑者,此時,前述超枝化聚合物與前述金屬微粒子以形成複合體較佳。
於此所謂複合體,係指藉由前述超枝化聚合物末端之銨基的作用,以接觸或近接金屬微粒子的狀態使兩者共存,而成為粒子狀之形態者,換言之,表現為具有前述超枝化聚合物之銨基附著或配位於金屬微粒子之構造的複合體。
據此,在本發明之「複合體」,並非僅為如上述般鍵結金屬微粒子與超枝化聚合物形成一個複合體者,而是亦可包含金屬微粒子與超枝化聚合物不形成鍵結部分,而分別獨立存在者。
具有銨基的超枝化聚合物與金屬微粒子之複合體的形成,係於包含超枝化聚合物與金屬微粒子之底塗
劑的調製時同時實施,作為該方法,有藉由低級銨配位子,製造某種程度穩定化之金屬微粒子後,藉由超枝化聚合物交換配位子之方法、或於具有銨基之超枝化聚合物的溶液中,藉由直接還原金屬離子,形成複合體之方法。例如,亦可藉由進行於溶解上述超枝化聚合物之溶液添加金屬鹽之水溶液,並對此溶液照射紫外線、或於該超枝化聚合物溶液添加金屬鹽之水溶液及還原劑等,還原金屬離子形成複合體。
在配位子交換法,成為原料之藉由低級銨配位子,經某種程度穩定化之金屬微粒子,可用Jounal of Organometallic Chemistry 1996,520,143-162等所記載之方法製造。可於所得之金屬微粒子的反應混合溶液,溶解具有銨基之超枝化聚合物,藉由室溫(約25℃)或加熱攪拌,得到成為目的之金屬微粒子複合體。
作為使用之溶劑,若為可將金屬微粒子與具有銨基的超枝化聚合物溶解成必要濃度以上之溶劑,雖並未特別限定,但具體而言,可列舉乙醇、n-丙醇、2-丙醇等之醇類;氯化亞甲基、氯仿等之鹵素化烴類;四氫呋喃(THF)、2-甲基四氫呋喃、四氫吡喃等之環狀醚類;乙腈、丁腈等之腈類等及此等之溶劑的混合液,較佳可列舉四氫呋喃。
混合金屬微粒子之反應混合液、與具有銨基的超枝化聚合物之溫度,通常可使用0℃~溶劑沸點的範圍,較佳為室溫(約25℃)~60℃的範圍。
尚,在配位子交換法,除了於胺系分散劑(低級銨配位子)以外,亦可藉由使用膦(Phosphine)系分散劑(膦配位子),某種程度預先穩定化金屬微粒子。
作為直接還原方法,將金屬離子與具有銨基之超枝化聚合物溶解於溶劑,藉由以甲醇、乙醇、2-丙醇、多元醇等之第一級或第二級醇類還原,可得到作為目的之金屬微粒子複合體。
作為於此所用之金屬離子源,可使用上述之金屬鹽。
作為使用之溶劑,若為可將金屬離子與具有銨基的超枝化聚合物溶解成必要濃度以上之溶劑,雖並未特別限定,但具體而言,可列舉甲醇、乙醇、丙醇、2-丙醇等之醇類;氯化亞甲基、氯仿等之鹵素化烴類;四氫呋喃(THF)、2-甲基四氫呋喃、四氫吡喃等之環狀醚類;乙腈、丁腈等之腈類;N,N-二甲基甲醯胺(DMF)、N-甲基-2-吡咯烷酮(NMP)等之醯胺類;二甲亞碸等之亞碸類等及此等之溶劑的混合液,較佳可列舉醇類、鹵素化烴類、環狀醚類,更佳可列舉乙醇、2-丙醇、氯仿、四氫呋喃等。
還原反應之溫度通常可使用0℃~溶劑沸點的範圍,較佳為室溫(約25℃)~60℃的範圍。
作為其他直接還原方法,將金屬離子與具有銨基之超枝化聚合物溶解於溶劑,藉由於氫氣體環境下進行反應,可得到作為目的之金屬微粒子複合體。
作為於此所用之金屬離子源,可使用上述之金屬鹽、或六羰基鉻[Cr(CO)6]、五羰基鐵[Fe(CO)5]、八羰基二鈷
[Co2(CO)8]、四羰基鎳[Ni(CO)4]等之金屬羰基錯合物。又亦可使用金屬烯烴錯合物或金屬膦錯合物、金屬氮錯合物等之0價金屬錯合物。
作為使用之溶劑,若為可將金屬離子與具有銨基的超枝化聚合物溶解成必要濃度以上之溶劑,雖並未特別限定,但具體而言,可列舉乙醇、丙醇等之醇類;氯化亞甲基、氯仿等之鹵素化烴類;四氫呋喃、2-甲基四氫呋喃、四氫吡喃等之環狀醚類;乙腈、丁腈等之腈類等及此等之溶劑的混合液,較佳可列舉四氫呋喃。混合金屬離子與具有銨基的超枝化聚合物之溫度,通常可使用0℃~溶劑沸點的範圍。
又,作為直接還原方法,將金屬離子與具有銨基之超枝化聚合物溶解於溶劑,藉由熱分解反應,可得到作為目的之金屬微粒子複合體。
作為於此所用之金屬離子源,可使用上述之金屬鹽或金屬羰基錯合物或其他0價之金屬錯合物、氧化銀等之金屬氧化物。
作為使用之溶劑,若為可將金屬離子與具有銨基的超枝化聚合物溶解成必要濃度以上之溶劑,雖並未特別限定,但具體而言,可列舉甲醇、乙醇、n-丙醇、2-丙醇、乙二醇等之醇類;氯化亞甲基、氯仿等之鹵素化烴類;四氫呋喃(THF)、2-甲基四氫呋喃、四氫吡喃等之環狀醚類;乙腈、丁腈等之腈類;苯、甲苯等之芳香族烴類等及此等之溶劑的混合液,較佳可列舉甲苯。
混合金屬離子與具有銨基的超枝化聚合物之溫度,通常可使用0℃~溶劑沸點的範圍,較佳為溶劑沸點附近,例如甲苯時為110℃(加熱迴流)。
如此進行所得之具有銨基的超枝化聚合物與金屬微粒子的複合體,經過再沉澱等之純化處理,可成為粉末等之固形物的形態。
本發明之底塗劑係包含前述(a)具有銨基的超枝化聚合物與(b)金屬微粒子(較佳為藉由此等所成之複合體)與前述(c)聚合性化合物與前述(d)光聚合起始劑,可為用在後述之[無電解鍍敷底塗層]的形成時之清漆的形態。
本發明之底塗劑可依必要藉由摻合增黏劑,調整底塗劑的黏度或流變特性。據此,增黏劑的添加,在將本發明之底塗劑作為印刷油墨使用時,可發揮特別重要的功能。
作為上述增黏劑,例如可列舉羧基乙烯基聚合物(Carbomer)等之聚丙烯酸類(亦包含交聯者);聚乙烯基吡咯烷酮(PVP)、聚乙烯基醇(PVA)、聚乙酸乙烯酯(PVAc)、聚苯乙烯(PS)等之乙烯基聚合物;聚氧化乙烯類;聚酯;聚碳酸酯;聚醯胺;聚胺基甲酸乙酯;澱粉糊精、寒天、卡拉膠、海藻酸、阿拉伯樹膠、瓜爾豆膠、黃蓍膠、刺槐豆膠、澱粉、果膠、羧基甲基纖維素、羥基乙基纖維素、羥基丙基纖維素等之多糖類;凝膠、酪蛋白等之蛋白質等。又,上述各聚合物中不僅均聚物亦包含共聚
物。此等增黏劑可一種單獨使用,又亦可併用二種以上。
本發明之底塗劑在不損害本發明的效果下,可進一步適當添加界面活性劑、各種表面調整劑、消泡劑等之添加劑。
作為上述界面活性劑,例如可列舉聚氧乙烯月桂醚、聚氧乙烯硬脂醚、聚氧乙烯十六烷醚、聚氧乙烯油醯醚等之聚氧乙烯烷醚類;聚氧乙烯辛基苯醚、聚氧乙烯壬基苯醚等之聚氧乙烯烷基芳醚類;聚氧乙烯.聚氧丙烯基嵌段共聚物類;去水山梨糖醇單月桂酸酯、去水山梨糖醇單棕櫚酸酯、去水山梨糖醇單硬脂酸酯、去水山梨糖醇單油酸酯、去水山梨糖醇三硬脂酸酯、去水山梨糖醇三油酸酯等之去水山梨糖醇脂肪酸酯類;聚氧乙烯去水山梨糖醇單月桂酸酯、聚氧乙烯去水山梨糖醇單棕櫚酸酯、聚氧乙烯去水山梨糖醇單硬脂酸酯、聚氧乙烯去水山梨糖醇三油酸酯等之聚氧乙烯非離子系界面活性劑;Eftop(註冊商標)EF-301、同EF-303、同EF-352[以上、三菱材料電子化成(股)製]、Megafac(註冊商標)F-171、同F-173、同R-08、同R-30[以上為DIC(股)製]、Novec(註冊商標)FC-430、同FC-431[以上為住友3M(股)製]、Asahi guard(註冊商標)AG-710[旭硝子(股)製]、Surflon(註冊商標)S-382[AGCSeimi Chemical(股)製]等之氟系界面活性劑等。
又,作為上述表面調整劑,可列舉信越矽(註
冊商標)KP-341[信越化學工業(股)製]等之矽系流平劑;BYK(註冊商標)-302、同307、同322、同323、同330、同333、同370、同375、同378[以上為畢克化學.日本(股)製]等之矽系表面調整劑等。
此等添加劑可一種單獨使用,又亦可併用二種以上。添加劑的使用量,相對於由前述超枝化聚合物與金屬微粒子所形成之複合體100質量份,較佳為0.001~50質量份,更佳為0.005~10質量,再更佳為0.01~5質量份。
上述之本發明之底塗劑,藉由塗佈於基材上進行光硬化,可形成無電解鍍敷底塗層。此無電解鍍敷底塗層亦為本發明之對象。
作為前述基材雖並未特別限定,但較佳可使用非導電性基材或導電性基材。
作為非導電性基材,例如可列舉玻璃、陶瓷等;聚乙烯樹脂、聚丙烯樹脂、氯化乙烯基樹脂、尼龍(聚醯胺樹脂)、聚醯亞胺樹脂、聚碳酸酯樹脂、丙烯酸樹脂、PEN(聚萘二甲酸乙二酯)樹脂、PET(聚對苯二甲酸乙二酯)樹脂、PEEK(聚醚醚酮)樹脂、ABS(丙烯腈-丁二烯-苯乙烯共聚物)樹脂、環氧樹脂、聚縮醛樹脂等;紙等。此等可適合在薄片或薄膜等之形態使用,對於此情況下之厚度並未特別限定。
又作為導電性基材,例如可列舉ITO(錫摻雜氧化銦)、或ATO(銻摻雜氧化錫)、FTO(氟摻雜氧化錫)、AZO(鋁摻雜氧化鋅)、GZO(鎵摻雜氧化鋅)、又各種不銹鋼、鋁以及杜拉鋁等之鋁合金、鐵以及鐵合金、銅以及黃銅、燐青銅、白銅及鈹銅等之銅合金、鎳以及鎳合金、以及銀以及德國銀等之銀合金等之金屬等。
進而,於上述非導電性基材上,以此等之導電性基材形成薄膜之基材亦可使用。又,上述基材可為三次元成形體。
作為由上述包含具有銨基的超枝化聚合物與金屬微粒子與聚合性化合物與光聚合起始劑之底塗劑,形成無電解鍍敷底塗層之具體方法,首先將前述具有銨基的超枝化聚合物與金屬微粒子(較佳為由此等所成之複合體)與聚合性化合物與光聚合起始劑,溶解或分散於適當溶劑而作為清漆的形態,將該清漆於形成金屬鍍敷被膜之基材上藉由旋塗法;刮刀塗佈法;浸塗法;輥塗法;棒塗佈法;模塗法;噴塗法;噴墨法;自來水筆奈米光微影(FPN)、Dip筆奈米光微影(DPN)等之筆光微影;活版印刷、柔版印刷、樹脂凸版印刷、接觸印刷、微接觸印刷(μCP)、奈米壓印光微影(NIL)、奈米轉印(nTP)等之凸版印刷法;凹版印刷、刻印等之凹版印刷法;平版印刷法;絲網印刷、滾筒油印機等之孔版印刷法;膠印印刷法等進行塗佈後,較佳為接著使溶劑蒸發.乾燥後,藉由照射紫外線等之活性光線使其光硬化,而形成薄層。
此等之塗佈方法當中,較佳為旋塗法、噴塗法、噴墨法、筆光微影、接觸印刷、μCP、NIL及nTP。使用旋塗法時,由於可於短時間塗佈,即使為揮發性高之溶液亦可利用,又,有可進行均勻性高之塗佈的優勢。使用噴塗法時,可用極少量之清漆進行均勻性高之塗佈,工業上非常有利。使用噴墨法、筆光微影、接觸印刷、μCP、NIL、nTP時,例如可有效率地形成(繪圖)配線等之微細圖型,工業上非常有利。
作為於此所使用之溶劑,若為溶解或分散上述複合體、聚合性化合物及光聚合起始劑者,則並未特別限定,例如可使用水;苯、甲苯、二甲苯、乙基苯、氯苯、二氯苯等之芳香族烴類;甲醇、乙醇、n-丙醇、2-丙醇、n-丁醇、2-丁醇、n-己醇、n-辛醇、2-辛醇、2-乙基己醇等之醇類;甲基溶纖劑、乙基溶纖劑、丁基溶纖劑、苯基溶纖劑等之溶纖劑類;丙二醇單甲醚(PGME)、丙二醇單乙醚、丙二醇單丁醚、二乙二醇單甲醚、二乙二醇單丁醚、二丙二醇單甲醚、三乙二醇單甲醚、三丙二醇單甲醚、乙二醇二甲醚、丙二醇二甲醚、二乙二醇二甲醚、二乙二醇二乙醚、二乙二醇二丁醚、二乙二醇乙基甲醚、二乙二醇丁基甲醚、二乙二醇異丙基甲醚、二丙二醇二甲醚、三乙二醇二甲醚、三丙二醇二甲醚等之甘醇醚類;乙二醇單甲醚乙酸酯、丙二醇單甲醚乙酸酯(PGMEA)等之甘醇酯類;四氫呋喃(THF)、甲基四氫呋喃、1,4-二噁烷、二乙醚等之醚類;乙酸乙酯、乙酸丁酯等之酯類;丙酮、
甲基乙基酮(MEK)、甲基異丁基酮(MIBK)、環戊酮、環己酮等之酮類;n-庚烷、n-己烷、環己烷等之脂肪族烴類;1,2-二氯乙烷、氯仿等之鹵素化脂肪族烴類;N-甲基-2-吡咯烷酮(NMP)、N,N-二甲基甲醯胺(DMF)、N,N-二甲基乙醯胺等之醯胺類;二甲亞碸等。此等溶劑可單獨使用,亦可混合2種以上的溶劑。進而,以調整清漆的黏度為目的,可添加乙二醇、丙二醇、丁二醇等之甘醇類。
又溶解或分散於上述溶劑的濃度雖為任意,但清漆中之前述複合體濃度為0.05~90質量%,較佳為0.1~80質量%。
又,作為上述噴墨法所用之溶劑,較佳為由水、一元醇及多元醇所構成之混合溶劑。
作為一元醇,例如可列舉甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基丙醇、2-甲基-2-丙醇、2-乙基己醇等之低級醇類;乙二醇單甲醚(甲基溶纖劑)、乙二醇單乙醚(乙基溶纖劑)、乙二醇單丙醚(丙基溶纖劑)、乙二醇單異丙醚(異丙基溶纖劑)、乙二醇單丁醚(丁基溶纖劑)、乙二醇單苯醚(苯基溶纖劑)等之乙二醇單烷醚類(溶纖劑類);丙二醇單甲醚(PGME)、丙二醇單乙醚、丙二醇單丙醚、丙二醇單丁醚、丙二醇單苯醚等之丙二醇單烷醚類;3-甲氧基丙醇、3-乙氧基丙醇、3-丙氧基丙醇、3-丁氧基丙醇、3-甲氧基丁醇、3-甲氧基-3-甲基丁醇、4-甲氧
基丁醇等之其他烷氧基醇類;二丙酮醇;乳酸甲酯、乳酸乙酯等之乳酸酯類等。此等之一元醇可一種單獨使用,亦可併用2種以上。
此等當中,較佳為低級醇類、二丙酮醇,更佳為1-丙醇、二丙酮醇。
作為多元醇,例如可列舉乙二醇;1,2-丙烷二醇(丙二醇)、1,3-丙烷二醇、2-甲基-1,3-丙烷二醇等之丙烷二醇類;1,2-丁二醇、1,3-丁二醇、1,4-丁二醇、2,3-丁二醇、2-甲基-1,4-丁二醇等之丁二醇類;1,5-戊二醇、3-甲基-1,5-戊二醇、2-甲基-2,4-戊二醇等之戊二醇類;1,6-己二醇等之己二醇類;甘油、1,2,6-己三醇等之三醇類等。此等之多元醇可一種單獨使用,亦可併用2種以上。
此等當中,較佳為丙烷二醇類、丁二醇類,更佳為1,2-丙烷二醇(丙二醇)、1,3-丙烷二醇、1,3-丁二醇、1,4-丁二醇。
作為此等較佳之組合,例如可列舉水/1-丙醇/乙二醇、水/1-丙醇/1,2-丙烷二醇(丙二醇)、水/1-丙醇/1,3-丙烷二醇、水/1-丙醇/1,3-丁二醇、水/1-丙醇/1,4-丁二醇、水/1-丙醇/2,3-丁二醇、水/1-丙醇/1,6-己二醇、水/二丙酮醇/乙二醇、水/二丙酮醇/1,2-丙烷二醇(丙二醇)、水/二丙酮醇/2-乙基己醇/乙二醇單苯醚(苯基溶纖劑)/1,2-丙烷二醇(丙二醇)、水/二丙酮醇/1,3-丙烷二醇、水/二丙酮
醇/1,3-丁二醇、水/二丙酮醇/1,4-丁二醇、水/二丙酮醇/2,3-丁二醇、水/甲醇/1,2-丙烷二醇(丙二醇)、水/乙醇/1,2-丙烷二醇(丙二醇)、水/2-丙醇/1,2-丙烷二醇(丙二醇)、水/1-丁醇/1,2-丙烷二醇(丙二醇)、水/2-丁醇/1,2-丙烷二醇(丙二醇)、水/2-甲基丙醇/1,2-丙烷二醇(丙二醇)、水/2-甲基-2-丙醇/1,2-丙烷二醇(丙二醇)等。
此等當中,更佳為水/1-丙醇/1,2-丙烷二醇(丙二醇)、水/1-丙醇/1,3-丙烷二醇、水/1-丙醇/1,3-丁二醇、水/1-丙醇/1,4-丁二醇、水/二丙酮醇/乙二醇、水/二丙酮醇/1,2-丙烷二醇(丙二醇)、水/二丙酮醇/2-乙基己醇/乙二醇單苯醚(苯基溶纖劑)/1,2-丙烷二醇(丙二醇)、水/二丙酮醇/1,3-丙烷二醇、水/二丙酮醇/1,3-丁二醇、水/二丙酮醇/1,4-丁二醇。
在上述混合溶劑之單醇的比例,較佳為5質量%以上且未滿80質量%、10質量%以上且未滿80質量%、20質量%以上且未滿70質量%、5質量%以上且未滿50質量%、20質量%以上且未滿40質量%。
又,在上述混合溶劑之多元醇的比例,較佳為5質量%以上且未滿50質量%,更佳為20質量%以上且未滿40質量%。
又溶解或分散於上述混合溶劑的濃度雖為任意,但清漆中之上述複合體濃度為0.05~10質量%,較佳為0.1~5質量%。
上述複合體的濃度未滿0.05質量%時,噴墨塗佈觸媒
油墨時,有易於產生斷線之虞,又複合體的濃度超過10質量%時,有產生噴墨噴嘴阻塞之虞。
作為溶劑之乾燥法,並非被特別限定者,例如使用熱板或烤箱,於適當環境下,亦即大氣、氮等之惰性氣體、真空中等使其蒸發即可。藉此,可得到具有均勻成膜面的底塗層。燒成溫度若為可使溶劑蒸發,雖並未特別限定,但較佳為於40~250℃進行。
作為光聚合所用之活性光線,例如可列舉紫外線、電子束、X光等。作為紫外線照射所用之光源,可使用太陽光線、化學燈、低壓水銀燈、高壓水銀燈、金屬鹵化物燈、氙氣燈、UV-LED等。又,光聚合後,依必要藉由進行後烘烤,具體而言,藉由使用熱板、烤箱等進行加熱,可使聚合完成。作為後烘烤之條件,雖並未特別限定,但通常於50~260℃、1~120分鐘的範圍進行。
藉由無電解鍍敷如上述進行所得之基材上所形成之無電解鍍敷底塗層,於無電解鍍敷底塗層之上形成金屬鍍敷膜。如此進行所得之金屬鍍敷膜、以及於基材上依序具備無電解鍍敷底塗層、金屬鍍敷膜之金屬被膜基材亦為本發明之對象。
無電解鍍敷處理(步驟)並未特別限定,可以一般所知之任何無電解鍍敷處理進行,例如一般而言係使用以往一般所知之無電解鍍敷液,於該鍍敷液(浴)浸漬形成於基材
上之無電解鍍敷底塗層之方法。
前述無電解鍍敷液作為主要,主要含有金屬離子(金屬鹽)、錯合劑、還原劑,配合其他用途可適當包含pH值調整劑、pH值緩衝劑、反應促進劑(第二錯合劑)、穩定劑、界面活性劑(對鍍敷膜之光澤賦予用途、被處理面之潤濕性改善用途等)等而成。
於此作為藉由無電解鍍敷所形成之金屬鍍敷膜所使用之金屬,例如可列舉鐵、鈷、鎳、銅、鈀、銀、錫、鉑、金及該等之合金,因應目的適當選擇。
又對於上述錯合劑、還原劑,因應金屬離子適當選擇即可。
又無電解鍍敷液可使用市售之鍍敷液,例如適合使用Meltex(股)製之無電解鎳鍍敷藥品(Melplate(註冊商標)NI系列)、無電解銅鍍敷藥品(Melplate(註冊商標)CU系列);奧野製藥工業(股)製之無電解鎳鍍敷液(ICPNikoron(註冊商標)系列、Top Piena650)、無電解銅鍍敷液(OPC-700無電解銅M-K、ATSAd CopperIW、同CT、OPCCopper(註冊商標)AF系列、同HFS、同NCA)、無電解錫鍍敷液(Sub-StarSN-5)、無電解金鍍敷液(Flash Gold330、Self GoldOTK-IT)、無電解銀鍍敷液(Muden Sliver);小島化學藥品(股)製之無電解鈀鍍敷液(PalletII)、無電解金鍍敷液(DipG系列、NCGold系列);佐佐木化學藥品(股)製之無電解銀鍍敷液(Esudaiya AG-40);日本Kanigen(股)製之無電解鎳鍍敷液(Schumer(註冊商標)系列、Schumer(註冊商
標)Kani Black(註冊商標)系列)、無電解鈀鍍敷液(S-KPD);陶氏化學公司製之無電解銅鍍敷液(Cuposit(註冊商標)Copper Mix系列、Circuposit(註冊商標)系列)、無電解鈀鍍敷液(Palamas(註冊商標)系列)、無電解鎳鍍敷液(DURAPOSIT(註冊商標)系列)、無電解金鍍敷液(AUROLECTROLESS(註冊商標)系列)、無電解錫鍍敷液(TINPOSIT(註冊商標)系列);上村工業(股)製之無電解銅鍍敷液(THRU-CUP(註冊商標)ELC-SP、同PSY、同PCY、同PGT、同PSR、同PEA、同PMK);Atotech日本(股)製之無電解銅鍍敷液(Printgant(註冊商標)PV、同PVE)等。
上述無電解鍍敷步驟係藉由調節鍍敷浴之溫度、pH值、浸漬時間、金屬離子濃度、攪拌之有無或攪拌速度、空氣.氧供給的有無或供給速度等,可調控金屬被膜之形成速度或膜厚。
以下,將本發明藉由實施例進一步具體說明,但並非藉此限定本發明者。在實施例,試料之物性測定係以下述之條件為根本使用下述之裝置進行。
裝置:東曹(股)製HLC-8220GPC
管柱:昭和電工(股)製Shodex(註冊商標)GPC KF-
804L+同KF-803L
管柱溫度:40℃
溶劑:四氫呋喃
檢測器:UV(254nm)、RI
裝置:日本電子(股)製JNM-L400
溶劑:CDCl3
基準峰值:四甲基矽烷(0.00ppm)
裝置:日本電子(股)製JNM-ECA700
溶劑:CDCl3
緩和試藥:三乙醯丙酮酸鉻(Cr(acac)3)
基準峰值:CDCl3(77.0ppm)
裝置:(股)島津製作所製ICPM-8500
裝置:(股)日立高新技術製H-8000
裝置:Eye Graphics(股)製US5-0401
裝置:Cluster technology(股)製Inkjet Designer
驅動器:Cluster technology(股)製WaveBuilder(註冊商標)PIJD-1SET
頭:Cluster technology(股)製PulseInjector(註冊商
標)PIJ-15NSET(噴嘴徑:15μm)
裝置:(股)Keyence製VHX-2000
又使用之簡稱係如以下所述。
HPS:超支化聚苯乙烯[日產化學工業(股)製Hyper Tech(註冊商標)HPS-200]
2EH:2-乙基己醇
DAA:二丙酮醇
IPA:2-丙醇
IPE:二異丙醚
PG:丙二醇
PhC:苯基溶纖劑
PrOH:1-丙醇
PEN:聚萘二甲酸乙二酯
4EG2A:四乙二醇二丙烯酸酯[日油(股)製BLEMMER(註冊商標)ADE-200]
14EG2A:十四乙二醇二丙烯酸酯[共榮社化學(股)製Light Acrylate 14EG-A]
DD2A:1,10-癸二醇二丙烯酸酯[新中村化學工業(股)製NK ester A-DOD-N]
DEAA:N,N-二乙基丙烯醯胺[KJChemicals(股)製DEAA(註冊商標)]
DP6A-12E:氧化乙烯改質二季戊四醇六丙烯酸酯(氧化乙烯加成莫耳數12)[新中村化學工業(股)製NK ester
A-DPH-12E]
EEEA:2-(2-乙氧基乙氧基)乙基丙烯酸酯[大阪有機化學工業(股)製Viscoat#190]
G3A-20E:氧化乙烯改質甘油三丙烯酸酯(氧化乙烯加成莫耳數20)[新中村化學工業(股)製NK ester A-GLY-20E]
LA:月桂基丙烯酸酯[日油(股)製BLEMMER(註冊商標)LA]
P4A-4E:氧化乙烯改質季戊四醇四丙烯酸酯(氧化乙烯加成莫耳數4)[新中村化學工業(股)製NK ester ATM-4E]
POEA:(2-苯氧基乙基)丙烯酸酯[大阪有機化學工業(股)製Viscoat#192]
UA4200:聚醚骨架2官能胺基甲酸乙酯丙烯酸酯[新中村化學工業(股)製NKOligoUA-4200]
UV7605B:6官能胺基甲酸乙酯丙烯酸酯[日本合成化學工業(股)製 紫光(註冊商標)UV-7605B]
8KX:(甲基)丙烯酸(甲基)丙烯酸酯[大成Fine chemical(股)製ACRIT8KX-078]
8UH:聚胺基甲酸乙酯(甲基)丙烯酸酯[大成Fine chemical(股)製ACRIT8UH-1006]
TPO:二苯基(2,4,6-三甲基苯甲醯基)膦氧化物[BASF日本(股)製IRGACURE(註冊商標)TPO]
NXZ:金屬皂系消泡劑[Sunnopco(股)製Nopco(註冊
商標)NXZ]
於500mL之反應燒瓶放入硫醯氯[岸田化學(股)製]27g及氯仿50g,進行攪拌使其均勻溶解。將此溶液於氮氣流下冷卻至0℃。
於另一300mL之反應燒瓶,放入於分子末端具有二硫代胺基甲酸酯基(Dithiocarbamate group)的超枝化聚合物HPS15g及氯仿150g,於氮氣流下攪拌至均勻為止。
於前述冷卻至0℃之硫醯氯/氯仿溶液中,在氮氣流下,從放入HPS/氯仿溶液之前述300mL反應燒瓶,使用送液泵,以反應液的溫度成為-5~5℃的方式耗費60分鐘加入該溶液。添加結束後,將反應液之溫度保持在-5~5℃並且攪拌6小時。
進而對此反應液,以反應液的溫度成為-5~5℃的方式,加入將環己烯[東京化成工業(股)製]16g溶解於氯仿
50g之溶液。添加結束後,將此反應液添加於IPA1,200g並使聚合物沉澱。濾取此沉澱,將所得之白色粉末溶解於氯仿100g,將此添加於IPA500g,使聚合物再沉澱。減壓過濾此沉澱物,進行真空乾燥,而得到作為白色粉末之於分子末端具有氯原子的超枝化聚合物(HPS-Cl)8.5g(收率99%)。
將所得之HPS-Cl之1H NMR光譜示於圖1。非常清楚從源自二硫代胺基甲酸酯基之峰值(4.0ppm、3.7ppm)消失,所得之HPS-Cl係HPS分子末端之二硫代胺基甲酸酯基幾乎全部被氯原子取代。又,藉由所得之HPS-Cl的GPC以聚苯乙烯換算測定之重量平均分子量Mw為14,000,分散度Mw/Mn為2.9。
於設置冷卻器之100mL反應燒瓶,放入製造例1所製造之HPS-Cl4.6g(30mmol)及氯仿15g,攪拌至均勻為止。對此溶液,加入將二甲基辛基胺[花王(股)製Firmin(註冊商標)DM0898]5.0g(31.5mmol)溶解於氯仿7.5g之溶液,進而加入IPA7.5g。將此混合物於氮環境下65℃
攪拌40小時。
冷卻至液溫30℃後,餾除溶劑。將所得之殘渣溶解於氯仿60g,將此溶液添加於IPE290g進行再沉澱純化。減壓過濾析出之聚合物,於50℃進行真空乾燥,而得到作為白色粉末之於分子末端具有二甲基辛基銨基的超枝化聚合物(HPS-N(Me)2OctCl)9.3g。
將所得之HPS-N(Me)2OctCl之13C NMR光譜示於圖2。非常清楚從苯環之峰值、與辛基末端之甲基的峰值,所得之HPS-N(Me)2OctCl係HPS-Cl分子末端之氯原子幾乎定量性被銨基取代。又,從HPS-Cl之Mw(14,000)及銨基導入率(100%)所算出HPS-N(Me)2OctCl的重量平均分子量Mw為28,000。
於設置冷卻器之500mL反應燒瓶,放入乙酸鈀[川研Fine chemical(股)製]4.6g及氯仿100g,並攪拌至均勻為止。對此溶液,把將於製造例2製造之HPS-N(Me)2OctCl5.0g溶解於氯仿100g之溶液,使用滴下漏斗加入。將此滴下漏斗內使用氯仿100g及乙醇100g,對前述反應燒瓶洗淨。將此混合物於氮環境下60℃攪拌14小時。
液溫冷卻至30℃後,餾除溶劑。將所得之殘渣溶解於氯仿38g及乙醇38g之混合液,將此溶液添加於IPE750g進行再沉澱純化。減壓過濾析出之聚合物,於50
℃進行真空乾燥,而得到作為黑色粉末之於分子末端具有銨基的超枝化聚合物與Pd粒子的複合體(Pd[HPS-N(Me)2OctCl])7.0g。
從ICP發光分析的結果,所得之Pd[HPS-N(Me)2OctCl]的Pd含量為31質量%。又,從TEM(透過型電子顯微鏡)圖像,該Pd粒子徑約為2~4nm。
使用市售之Printgant(註冊商標)PV[Atotech日本(股)製],如以下般調整無電解銅鍍敷液。
於200mL之燒瓶,放入純水178mL、Basic Printgant V15mL、Copper solution Printgant VE 2mL、Starter Printgant PV 1.2mL、Stabilizer Printgant PV 0.2mL、還原劑Cu 3.2mL、及NaOH 0.52g,進行攪拌並昇溫至40℃,以作為無電解銅鍍敷液。
混合以下之各成分,調製超枝化聚合物-Pd粒子複合體(HBP-Pd)濃度1質量%的無電解鍍敷底塗劑。
(1)HBP-Pd:Pd[HPS-N(Me)2OctCl]100質量份
(2)聚合性化合物:表1所記載之化合物 表1所記載的量
(3)光聚合起始劑:TPO相對於聚合性化合物為3質量份
(4)溶劑:水-PrOH-PG混合溶液(質量比1:1:1)(1)~(4)的總量成為10,000質量份的量
將上述底塗劑旋塗(200rpm×5秒接著2,000rpm×30秒)於PEN薄膜(50×50mm)易接著面上。將此基材於80℃之熱板1分鐘,接著於150℃之熱板乾燥5分鐘,得到於基材上全面具備底塗層之基材。將所得之底塗層於空氣環境下,藉由照射曝光量800mJ/cm2之UV光來進行曝光而硬化。
將所得之基材浸漬10分鐘於已加熱至40℃之參考例1調製之無電解銅鍍敷液中。然後,水洗取出之基材,藉由於120℃之熱板乾燥10分鐘,而得到鍍敷基材。
又,於其他PEN薄膜無處理面上藉由上述方法,而得到實施鍍敷之基材。
對於此等之鍍敷基材上之金屬鍍敷膜,分別評估基材密著性。對於基材密著性,於所得之鍍敷基材上之金屬鍍敷膜部分,貼上寬18mm之黏著膠帶[Nichiban(股)製 透明膠帶(註冊商標)CT-18S],以手指強力擦拭使其牢牢密著後,一口氣剝離密著之黏著膠帶,將金屬鍍敷膜的狀態依照以下之基準,以目視評估。將結果合併示於表1。
A:無法確認金屬鍍敷膜之剝離密著於基材上
B:部分剝離金屬鍍敷膜
C:密著黏著膠帶的部分約三成以上的金屬鍍敷膜剝離附著於黏著膠帶
進而除了(5)作為消泡劑之NXZ摻合5質量份,(4)溶劑係將水-DAA-2EH-PhC-PG混合溶液(質量比5:64:5:1:25)變更為(1)~(5)總量成為10,000質量份的量之外,其他與實施例1進行同樣操作、評估。將結果合併示於表1。
除了未添加聚合性化合物及光聚合起始劑之外,其他與實施例1進行同樣操作、評估。將結果合併示於表1。
如表1所示,於使用本發明之底塗劑形成之
鍍敷膜(實施例1~12),確認在PEN薄膜之易接著面密著性皆優異。進而在實施例5、6、8、11、14、15,成為即使無處理面密著性亦高之結果。
對此,於未包含聚合性化合物之底塗劑(比較例1),無論是PEN之易接著面或無處理面皆無密著性。
由以上之結果,確認藉由使用本發明之底塗劑,得到密著性優異之鍍敷膜。
將於實施例11調製之底塗劑使用噴墨系統,以驅動波形:A、重複頻率數:1.3kHz、階段速度:20mm/秒、液滴間隔15μm,於PEN薄膜易接著面上,將長度30mm之細線以100μm間隔繪圖10條。尚,驅動電壓係以觀察液滴的飛行並且不引起液滴彎曲的方式以4~6V調整。
將繪圖上述之細線之薄膜於80℃之熱板1分鐘,接著於150℃之熱板乾燥5分鐘,而得到於基材上具備細線形狀之底塗層之基材。將所得之底塗層於空氣環境下,藉由照射曝光量800mJ/cm2之UV光進行曝光而硬化。
將所得之基材浸漬10分鐘於已加熱至40℃之參考例1調製之無電解銅鍍敷液中。然後,水洗取出之基材,藉由於120℃之熱板乾燥10分鐘,而得到鍍敷基材。
對於所得之經無電解鍍敷處理之基材的銅鍍敷圖型,觀察數位顯微鏡圖像時,確認為平均線寬29μm之直線度高的細線圖型。
Claims (16)
- 一種光硬化性底塗劑,其係於基材上藉由無電解鍍敷處理,用以形成金屬鍍敷膜之底塗劑,其係包含:(a)於分子末端具有銨基且重量平均分子量為1,000~5,000,000之超枝化聚合物(Hyperbranched polymer)、(b)金屬微粒子、(c)具有(甲基)丙烯醯基之聚合性化合物、及(d)光聚合起始劑。
- 如請求項1之光硬化性底塗劑,其中,前述(c)聚合性化合物係具有(甲基)丙烯醯基,且為具有選自由氧伸烷基構造、胺基甲酸乙酯構造及聚(甲基)丙烯酸構造所構成之群組中之至少一個構造的化合物。
- 如請求項1之光硬化性底塗劑,其中,前述(c)聚合性化合物係具有(甲基)丙烯醯基,且為具有選自由氧伸烷基構造及胺基甲酸乙酯構造所構成之群組中之至少一個構造的化合物。
- 如請求項2之光硬化性底塗劑,其中,前述(c)聚合性化合物係具有(甲基)丙烯醯基,且為具有氧伸烷基構造的化合物。
- 如請求項2之光硬化性底塗劑,其中,前述(c)聚合性化合物為胺基甲酸乙酯(甲基)丙烯酸酯化合物。
- 如請求項2之光硬化性底塗劑,其中,前述(c)聚合性化合物為具有(甲基)丙烯醯基之聚(甲基)丙烯酸化合物。
- 如請求項1~請求項6中任一項之光硬化性底塗劑,其中,前述(c)聚合性化合物係於分子內具有2個以上(甲基)丙烯醯基之化合物。
- 如請求項1~請求項7中任一項之光硬化性底塗劑,其中,前述(a)超枝化聚合物為式[1]表示之超枝化聚合物;
- 如請求項8之光硬化性底塗劑,其中,前述(a)超枝化聚合物為式[3]表示之超枝化聚合物;
- 如請求項1~請求項9中任一項之光硬化性底塗劑,其中,前述(b)金屬微粒子係選自由鐵(Fe)、鈷(Co)、鎳(Ni)、銅(Cu)、鈀(Pd)、銀(Ag)、錫(Sn)、鉑(Pt)及金(Au)所構成之群組中之至少一種金屬的微粒子。
- 如請求項10之光硬化性底塗劑,其中,前述(b)金屬微粒子為鈀微粒子。
- 如請求項1~請求項11中任一項之光硬化性底塗劑,其中,前述(b)金屬微粒子為具有1~100nm之平均粒徑的微粒子。
- 一種無電解鍍敷底塗層,其係將如請求項1~請求項12中任一項之光硬化性底塗劑藉由光硬化進行層形成而得到。
- 一種金屬鍍敷膜,其係藉由於如請求項13之無電解鍍敷底塗層進行無電解鍍敷,而形成於該底塗層上。
- 一種金屬被膜基材,其係具備基材、與形成於該基材上之如請求項13之無電解鍍敷底塗層、與形成於該無電解鍍敷底塗層上之如請求項14之金屬鍍敷膜。
- 一種金屬被膜基材的製造方法,其係包含下述A步驟~C步驟;A步驟:將如請求項1~請求項12中任一項之光硬化性底塗劑塗佈於基材上,形成塗膜之步驟、B步驟:將塗佈了光硬化性底塗劑之基材曝光,形成底塗層之步驟、C步驟:將具備底塗層之基材浸漬於無電解鍍敷浴,形成金屬鍍敷膜之步驟。
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