JP5916482B2 - Photosensitive conductive paste and conductive circuit - Google Patents
Photosensitive conductive paste and conductive circuit Download PDFInfo
- Publication number
- JP5916482B2 JP5916482B2 JP2012080921A JP2012080921A JP5916482B2 JP 5916482 B2 JP5916482 B2 JP 5916482B2 JP 2012080921 A JP2012080921 A JP 2012080921A JP 2012080921 A JP2012080921 A JP 2012080921A JP 5916482 B2 JP5916482 B2 JP 5916482B2
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- acid
- carbon atoms
- conductive
- photosensitive
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- -1 oxime ester Chemical class 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 23
- UVZICZIVKIMRNE-UHFFFAOYSA-N thiodiacetic acid Chemical compound OC(=O)CSCC(O)=O UVZICZIVKIMRNE-UHFFFAOYSA-N 0.000 claims description 18
- 239000011230 binding agent Substances 0.000 claims description 15
- 239000003999 initiator Substances 0.000 claims description 15
- 239000000178 monomer Substances 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 description 51
- 125000000217 alkyl group Chemical group 0.000 description 39
- 229920005989 resin Polymers 0.000 description 20
- 239000011347 resin Substances 0.000 description 20
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 19
- 239000011248 coating agent Substances 0.000 description 18
- 238000000576 coating method Methods 0.000 description 18
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 17
- 150000001875 compounds Chemical class 0.000 description 13
- 238000011161 development Methods 0.000 description 13
- 230000018109 developmental process Effects 0.000 description 13
- 238000000034 method Methods 0.000 description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 239000002253 acid Substances 0.000 description 9
- 125000005843 halogen group Chemical group 0.000 description 9
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 9
- 239000000758 substrate Substances 0.000 description 8
- 125000003545 alkoxy group Chemical group 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 150000008065 acid anhydrides Chemical class 0.000 description 6
- 125000003710 aryl alkyl group Chemical group 0.000 description 6
- 125000003118 aryl group Chemical group 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 150000007519 polyprotic acids Polymers 0.000 description 6
- 125000002252 acyl group Chemical group 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 5
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 description 5
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 5
- 125000004430 oxygen atom Chemical group O* 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 125000003282 alkyl amino group Chemical group 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 4
- 125000000753 cycloalkyl group Chemical group 0.000 description 4
- 125000004663 dialkyl amino group Chemical group 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 4
- 239000003208 petroleum Substances 0.000 description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 4
- 238000007650 screen-printing Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000012719 thermal polymerization Methods 0.000 description 4
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 description 3
- 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
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 244000028419 Styrax benzoin Species 0.000 description 3
- 235000000126 Styrax benzoin Nutrition 0.000 description 3
- 235000008411 Sumatra benzointree Nutrition 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 229960002130 benzoin Drugs 0.000 description 3
- 230000015572 biosynthetic process Effects 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
- 238000013461 design Methods 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 235000019382 gum benzoic Nutrition 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000059 patterning Methods 0.000 description 3
- 238000000016 photochemical curing Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000002685 polymerization catalyst Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 125000001424 substituent group Chemical group 0.000 description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 3
- BTJPUDCSZVCXFQ-UHFFFAOYSA-N 2,4-diethylthioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC(CC)=C3SC2=C1 BTJPUDCSZVCXFQ-UHFFFAOYSA-N 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 description 2
- LEJBBGNFPAFPKQ-UHFFFAOYSA-N 2-(2-prop-2-enoyloxyethoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOC(=O)C=C LEJBBGNFPAFPKQ-UHFFFAOYSA-N 0.000 description 2
- INQDDHNZXOAFFD-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOC(=O)C=C INQDDHNZXOAFFD-UHFFFAOYSA-N 0.000 description 2
- 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 2
- NJWGQARXZDRHCD-UHFFFAOYSA-N 2-methylanthraquinone Chemical compound C1=CC=C2C(=O)C3=CC(C)=CC=C3C(=O)C2=C1 NJWGQARXZDRHCD-UHFFFAOYSA-N 0.000 description 2
- QCAHUFWKIQLBNB-UHFFFAOYSA-N 3-(3-methoxypropoxy)propan-1-ol Chemical compound COCCCOCCCO QCAHUFWKIQLBNB-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
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 2
- 241000282994 Cervidae Species 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
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 125000002947 alkylene group Chemical group 0.000 description 2
- 239000012965 benzophenone Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 125000004386 diacrylate group Chemical group 0.000 description 2
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 description 2
- 238000005227 gel permeation chromatography Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 125000001624 naphthyl group Chemical group 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000000206 photolithography Methods 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- UOHMMEJUHBCKEE-UHFFFAOYSA-N prehnitene Chemical compound CC1=CC=C(C)C(C)=C1C UOHMMEJUHBCKEE-UHFFFAOYSA-N 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 description 1
- 125000004209 (C1-C8) alkyl group Chemical group 0.000 description 1
- XKSUVRWJZCEYQQ-UHFFFAOYSA-N 1,1-dimethoxyethylbenzene Chemical compound COC(C)(OC)C1=CC=CC=C1 XKSUVRWJZCEYQQ-UHFFFAOYSA-N 0.000 description 1
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical compound CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 description 1
- SUDVPELGFZKOMD-UHFFFAOYSA-N 1,2-di(propan-2-yl)thioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=C(C(C)C)C(C(C)C)=CC=C3SC2=C1 SUDVPELGFZKOMD-UHFFFAOYSA-N 0.000 description 1
- MSAHTMIQULFMRG-UHFFFAOYSA-N 1,2-diphenyl-2-propan-2-yloxyethanone Chemical compound C=1C=CC=CC=1C(OC(C)C)C(=O)C1=CC=CC=C1 MSAHTMIQULFMRG-UHFFFAOYSA-N 0.000 description 1
- QWOZZTWBWQMEPD-UHFFFAOYSA-N 1-(2-ethoxypropoxy)propan-2-ol Chemical compound CCOC(C)COCC(C)O QWOZZTWBWQMEPD-UHFFFAOYSA-N 0.000 description 1
- GPRYKVSEZCQIHD-UHFFFAOYSA-N 1-(4-aminophenyl)ethanone Chemical compound CC(=O)C1=CC=C(N)C=C1 GPRYKVSEZCQIHD-UHFFFAOYSA-N 0.000 description 1
- BOCJQSFSGAZAPQ-UHFFFAOYSA-N 1-chloroanthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2Cl BOCJQSFSGAZAPQ-UHFFFAOYSA-N 0.000 description 1
- JCTXKRPTIMZBJT-UHFFFAOYSA-N 2,2,4-trimethylpentane-1,3-diol Chemical compound CC(C)C(O)C(C)(C)CO JCTXKRPTIMZBJT-UHFFFAOYSA-N 0.000 description 1
- CERJZAHSUZVMCH-UHFFFAOYSA-N 2,2-dichloro-1-phenylethanone Chemical compound ClC(Cl)C(=O)C1=CC=CC=C1 CERJZAHSUZVMCH-UHFFFAOYSA-N 0.000 description 1
- GIMQKKFOOYOQGB-UHFFFAOYSA-N 2,2-diethoxy-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(OCC)(OCC)C(=O)C1=CC=CC=C1 GIMQKKFOOYOQGB-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
- LCHAFMWSFCONOO-UHFFFAOYSA-N 2,4-dimethylthioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(C)=CC(C)=C3SC2=C1 LCHAFMWSFCONOO-UHFFFAOYSA-N 0.000 description 1
- XVGDJNZHNCJHIP-UHFFFAOYSA-N 2-(1-carboxyethylsulfanyl)propanoic acid Chemical compound OC(=O)C(C)SC(C)C(O)=O XVGDJNZHNCJHIP-UHFFFAOYSA-N 0.000 description 1
- GNKPXNIWNNKLAA-UHFFFAOYSA-N 2-(1-cyanoethyldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)N=NC(C)(C)C#N GNKPXNIWNNKLAA-UHFFFAOYSA-N 0.000 description 1
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 1
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 1
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-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
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- WFSMVVDJSNMRAR-UHFFFAOYSA-N 2-[2-(2-ethoxyethoxy)ethoxy]ethanol Chemical compound CCOCCOCCOCCO WFSMVVDJSNMRAR-UHFFFAOYSA-N 0.000 description 1
- FDSUVTROAWLVJA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OCC(CO)(CO)COCC(CO)(CO)CO FDSUVTROAWLVJA-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
- NQBXSWAWVZHKBZ-UHFFFAOYSA-N 2-butoxyethyl acetate Chemical compound CCCCOCCOC(C)=O NQBXSWAWVZHKBZ-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
- KMNCBSZOIQAUFX-UHFFFAOYSA-N 2-ethoxy-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(OCC)C(=O)C1=CC=CC=C1 KMNCBSZOIQAUFX-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
- SJEBAWHUJDUKQK-UHFFFAOYSA-N 2-ethylanthraquinone Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC=C3C(=O)C2=C1 SJEBAWHUJDUKQK-UHFFFAOYSA-N 0.000 description 1
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 description 1
- BQZJOQXSCSZQPS-UHFFFAOYSA-N 2-methoxy-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(OC)C(=O)C1=CC=CC=C1 BQZJOQXSCSZQPS-UHFFFAOYSA-N 0.000 description 1
- YTPSFXZMJKMUJE-UHFFFAOYSA-N 2-tert-butylanthracene-9,10-dione Chemical compound C1=CC=C2C(=O)C3=CC(C(C)(C)C)=CC=C3C(=O)C2=C1 YTPSFXZMJKMUJE-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Conductive Materials (AREA)
- Materials For Photolithography (AREA)
- Parts Printed On Printed Circuit Boards (AREA)
Description
本発明は、基板に導電回路を形成する感光性導電ペーストおよびそれを用いた導電回路に関する。 The present invention relates to a photosensitive conductive paste for forming a conductive circuit on a substrate and a conductive circuit using the same.
近年、高集積化されたLSIや各種の電子部品を多数搭載するための多層回路基板、或いはプラズマディスプレイパネル（以下「PDP」ともいう。）などのフラットパネルディスプレイ（以下「FPD」ともいう。）において、小型化、高密度化、高精細化等の要求が高まっており、これらに形成される回路や電極等のファイン化が従来にも増して求められるようになってきている。 In recent years, a highly integrated LSI and a multilayer circuit board for mounting a large number of various electronic components, or a flat panel display (hereinafter also referred to as “FPD”) such as a plasma display panel (hereinafter also referred to as “PDP”). However, there is an increasing demand for downsizing, high density, high definition, etc., and finer circuit and electrodes formed on these are increasingly required.
導電回路を形成する方法として、有機バインダーに導電性粉末を混合した非感光性の導電ペーストを用い、スクリーン印刷等の印刷技術を利用した回路形成方法が広く知られている（例えば特許文献1など参照）。しかしながら、スクリーン印刷では、工業的に安定して100μｍ以下の線幅を有する導体パターンを形成することが困難であり、作成可能なファインパターンには限界があった。また、印刷マスクが大きくなるとマスクパターンの寸法誤差が大きくなるため、例えば30インチ以上のPDPの場合、高精細のPDPの生産は技術的に困難となっている。 As a method of forming a conductive circuit, a circuit forming method using a printing technique such as screen printing using a non-photosensitive conductive paste in which conductive powder is mixed in an organic binder is widely known (for example, Patent Document 1) reference). However, in screen printing, it is difficult to form a conductor pattern having a line width of 100 μm or less in an industrially stable manner, and there are limits to the fine patterns that can be created. Further, since the dimensional error of the mask pattern increases as the printing mask becomes larger, for example, in the case of a PDP of 30 inches or more, production of a high-definition PDP is technically difficult.
これに対し、100μｍ以下の線幅を有する導電回路を形成する方法として、感光性の導電ペーストを用い、フォトリソグラフィー技術を利用して基材上に導電回路を形成する方法が知られている（例えば特許文献2など参照）。この手法によれば、スクリーン印刷を利用した場合に比べ、高精細な導電回路を形成することができる。 On the other hand, as a method of forming a conductive circuit having a line width of 100 μm or less, a method of forming a conductive circuit on a substrate using a photosensitive conductive paste and utilizing a photolithography technique is known ( For example, see Patent Document 2). According to this method, a high-definition conductive circuit can be formed as compared with the case where screen printing is used.
一方、導電回路を低抵抗とするにはペースト中の導電性粉末の含有比率を上げる必要がある。しかしながら、フォトリソグラフィー技術を利用した手法では、導電性粉末によって塗膜の内部（深部）にまで硬化が十分に行われにくく、照射光を長時間照射する必要があり、これにより反応で生成したラジカルや活性種の拡散が進んでしまい導電回路の解像性が低下するという問題があった。 On the other hand, to reduce the resistance of the conductive circuit, it is necessary to increase the content ratio of the conductive powder in the paste. However, in the technique using the photolithography technique, it is difficult to sufficiently cure the inside (deep part) of the coating film by the conductive powder, and it is necessary to irradiate irradiation light for a long time, and thus the radical generated by the reaction. In addition, there is a problem that the diffusion of the active species proceeds and the resolution of the conductive circuit is lowered.
本発明は、上記課題を解決するためになされたものであり、その目的は、解像性が高く、且つ低抵抗の導電回路の形成に適した感光性導電ペーストを提供することにある。 The present invention has been made to solve the above-described problems, and an object of the present invention is to provide a photosensitive conductive paste having high resolution and suitable for forming a low-resistance conductive circuit.
本実施形態に係る感光性導電ペーストは、有機バインダーと、導電性粉末と、光重合成モノマーと、オキシムエステル係光重合開始剤と、チオジグリコール酸およびチオジグリコール酸の誘導体の少なくとも何れか１種とを含有することを特徴としている。このような構成により、高解像度であり且つ低抵抗の導電回路を形成することができる。また、上記導電性粉末に銀粉を含有していることが好ましい。また、導電回路の形成にこれらの感光性導電ペーストを用いることを特徴としている。 The photosensitive conductive paste according to this embodiment includes at least one of an organic binder, conductive powder, a photopolymerization monomer, an oxime ester-related photopolymerization initiator, thiodiglycolic acid and a derivative of thiodiglycolic acid. It is characterized by containing 1 type. With such a structure, a high-resolution and low-resistance conductive circuit can be formed. Moreover, it is preferable that the said conductive powder contains silver powder. Further, these photosensitive conductive pastes are used for forming a conductive circuit.
本発明にかかる感光性導電ペーストによれば、高解像、且つ低抵抗の導電回路を形成することができる。 According to the photosensitive conductive paste of the present invention, a high-resolution and low-resistance conductive circuit can be formed.
本発明の発明者らは、上記課題に対し、鋭意検討した結果、導電回路形成に用いるペーストに、有機バインダーと、導電性粉末と、光重合性モノマーと、オキシムエステル系光重合開始剤と、チオジグリコール酸およびチオジグリコール酸の誘導体の少なくとも何れか１種とを含有することで、解像性が高く、且つ低抵抗の導電回路を形成できることを見出した。
即ち、導電回路形成に用いる感光性導電ペースト中に光重合開始剤としてオキシムエステル系光重合開始剤を含有させることにより高解像化を図ると共に、さらにこれに、チオジグリコール酸およびチオジグリコール酸の誘導体の少なくとも何れか１種を含有させることによって低抵抗化も図れることを見出し、本発明を完成するに至った。
以下、本実施形態の感光性導電ペーストについて詳細に説明する。
The inventors of the present invention, as a result of intensive investigations on the above problems, in a paste used for forming a conductive circuit, an organic binder, a conductive powder, a photopolymerizable monomer, an oxime ester photopolymerization initiator, It has been found that a conductive circuit having high resolution and low resistance can be formed by containing at least one of thiodiglycolic acid and thiodiglycolic acid derivatives.
That is, by incorporating an oxime ester photopolymerization initiator as a photopolymerization initiator in a photosensitive conductive paste used for forming a conductive circuit, high resolution is achieved, and thiodiglycolic acid and thiodiglycol are further added thereto. It has been found that the resistance can be reduced by containing at least one of acid derivatives, and the present invention has been completed.
Hereinafter, the photosensitive conductive paste of this embodiment will be described in detail.
本実施形態の感光性導電ペーストにおける有機バインダーは、導電性粉末を分散し、基板上に塗布可能な状態とし、また、パターン露光により現像することにより、塗膜にパターンを形成するために用いられる。 The organic binder in the photosensitive conductive paste of the present embodiment is used to form a pattern on a coating film by dispersing conductive powder so that it can be applied onto a substrate and developing it by pattern exposure. .
有機バインダーとしては、カルボキシル基を有する樹脂、具体的にはそれ自体がエチレン性二重結合を有するカルボキシル基含有感光性樹脂およびエチレン性不飽和二重結合を有さないカルボキシル基含有樹脂のいずれも使用可能である。好適に使用できる樹脂（オリゴマーおよびポリマーのいずれでもよい）としては、以下のようなものが挙げられる。 As the organic binder, a carboxyl group-containing resin, specifically, a carboxyl group-containing photosensitive resin that itself has an ethylenic double bond and a carboxyl group-containing resin that does not have an ethylenically unsaturated double bond. It can be used. Examples of the resin (which may be either an oligomer or a polymer) that can be suitably used include the following.
（１）（メタ）アクリル酸などの不飽和カルボン酸と、メチル（メタ）アクリレートなどの不飽和二重結合を有する化合物を共重合させることによって得られるカルボキシル基含有樹脂。
（２）（メタ）アクリル酸などの不飽和カルボン酸と、メチル（メタ）アクリレートなどの不飽和二重結合を有する化合物の共重合体に、グリシジル（メタ）アクリレートや（メタ）アクリル酸クロライドなどにより、エチレン性不飽和基をペンダントとして付加させることによって得られるカルボキシル基含有感光性樹脂。
（３）グリシジル（メタ）アクリレートなどのエポキシ基と不飽和二重結合を有する化合物と、メチル（メタ）アクリレートなどの不飽和二重結合を有する化合物の共重合体に、（メタ）アクリル酸などの不飽和カルボン酸を反応させ、生成した２級の水酸基にテトラヒドロフタル酸無水物などの多塩基酸無水物を反応させて得られるカルボキシル基含有感光性樹脂。
（４）無水マレイン酸などの不飽和二重結合を有する酸無水物と、スチレンなどの不飽和二重結合を有する化合物の共重合体に、２−ヒドロキシエチル（メタ）アクリレートなどの水酸基と不飽和二重結合を有する化合物を反応させて得られるカルボキシル基含有感光性樹脂。
（５）多官能エポキシ化合物と（メタ）アクリル酸などの不飽和カルボン酸を反応させ、生成した２級の水酸基にテトラヒドロフタル酸無水物などの多塩基酸無水物を反応させて得られるカルボキシル基含有感光性樹脂。
（６）メチル（メタ）アクリレートなどの不飽和二重結合を有する化合物とグリシジル（メタ）アクリレートの共重合体のエポキシ基に、１分子中に１つのカルボキシル基を有し、エチレン性不飽和結合を持たない有機酸を反応させ、生成した２級の水酸基に多塩基酸無水物を反応させて得られるカルボキシル基含有感光性樹脂。
（７）ポリビニルアルコールなどの水酸基含有ポリマーに多塩基酸無水物を反応させて得られるカルボキシル基含有樹脂。
（８）ポリビニルアルコールなどの水酸基含有ポリマーに、テトラヒドロフタル酸無水物などの多塩基酸無水物を反応させて得られるカルボキシル基含有樹脂に、グリシジル（メタ）アクリレートなどのエポキシ基と不飽和二重結合を有する化合物をさらに反応させて得られるカルボキシル基含有感光性樹脂。
(1) A carboxyl group-containing resin obtained by copolymerizing an unsaturated carboxylic acid such as (meth) acrylic acid and a compound having an unsaturated double bond such as methyl (meth) acrylate.
(2) A copolymer of an unsaturated carboxylic acid such as (meth) acrylic acid and a compound having an unsaturated double bond such as methyl (meth) acrylate, glycidyl (meth) acrylate, (meth) acrylic acid chloride, etc. A carboxyl group-containing photosensitive resin obtained by adding an ethylenically unsaturated group as a pendant.
(3) A copolymer of an epoxy group such as glycidyl (meth) acrylate and an unsaturated double bond and a compound having an unsaturated double bond such as methyl (meth) acrylate, (meth) acrylic acid, etc. A carboxyl group-containing photosensitive resin obtained by reacting an unsaturated carboxylic acid of the above and reacting the resulting secondary hydroxyl group with a polybasic acid anhydride such as tetrahydrophthalic anhydride.
(4) To a copolymer of an acid anhydride having an unsaturated double bond such as maleic anhydride and a compound having an unsaturated double bond such as styrene, a hydroxyl group such as 2-hydroxyethyl (meth) acrylate and A carboxyl group-containing photosensitive resin obtained by reacting a compound having a saturated double bond.
(5) A carboxyl group obtained by reacting a polyfunctional epoxy compound with an unsaturated carboxylic acid such as (meth) acrylic acid, and reacting the resulting secondary hydroxyl group with a polybasic acid anhydride such as tetrahydrophthalic anhydride. Contains photosensitive resin.
(6) An epoxy group of a copolymer of an unsaturated double bond such as methyl (meth) acrylate and a glycidyl (meth) acrylate has one carboxyl group in one molecule, and an ethylenically unsaturated bond A carboxyl group-containing photosensitive resin obtained by reacting an organic acid having no carboxylic acid, and reacting the resulting secondary hydroxyl group with a polybasic acid anhydride.
(7) A carboxyl group-containing resin obtained by reacting a polybasic acid anhydride with a hydroxyl group-containing polymer such as polyvinyl alcohol.
(8) A carboxyl group-containing resin obtained by reacting a hydroxyl group-containing polymer such as polyvinyl alcohol with a polybasic acid anhydride such as tetrahydrophthalic anhydride, an epoxy group such as glycidyl (meth) acrylate, and an unsaturated double group. A carboxyl group-containing photosensitive resin obtained by further reacting a compound having a bond.
これらのうち、特に（１）、（２）、（３）、（６）の樹脂が好適に用いられる。また、これらの樹脂は単独または混合して用いることができる。
なお、本明細書中の（メタ）アクリレートとは、アクリレート、メタクリレートおよびそれらの混合物を総称する用語であり、他の類似の表現についても同様とする。
Of these, the resins (1), (2), (3), and (6) are particularly preferably used. These resins can be used alone or in combination.
In addition, (meth) acrylate in this specification is a term which generically refers to acrylate, methacrylate and a mixture thereof, and the same applies to other similar expressions.
このような有機バインダーの配合量としては、不揮発成分（乾燥工程でペースト中から揮発せず、膜に残存する成分）を基準として、１〜５０質量％で配合されることが好ましい。１質量％未満の場合、形成する塗膜中のこれら樹脂の不足により、現像性が大幅に悪化し、現像によるパターニングが困難となる。一方、５０質量％を超えた場合、導電性粉末の割合が不足し、抵抗値が悪化する傾向にある。 The amount of such an organic binder is preferably 1 to 50% by mass based on the nonvolatile component (the component that does not volatilize from the paste in the drying step and remains in the film). When the amount is less than 1% by mass, developability is greatly deteriorated due to the lack of these resins in the coating film to be formed, and patterning by development becomes difficult. On the other hand, when it exceeds 50 mass%, the ratio of the conductive powder is insufficient, and the resistance value tends to deteriorate.
また、重量平均分子量としては、１，０００〜１００，０００であることが好ましい。重量平均分子量が１，０００未満の場合、現像時の塗膜の密着性が劣化し、一方、１００，０００を超えた場合、現像不良を生じやすくなる。より好ましくは５，０００〜７０，０００である。なお、重量平均分子量は、ゲルパーミエーションクロマトグラフィー（GPC）で測定したポリスチレン換算の値である。 Moreover, as a weight average molecular weight, it is preferable that it is 1,000-100,000. When the weight average molecular weight is less than 1,000, the adhesion of the coating film at the time of development is deteriorated. More preferably, it is 5,000-70,000. The weight average molecular weight is a value in terms of polystyrene measured by gel permeation chromatography (GPC).
また、用いられる有機バインダーの酸価は、５０〜２５０mgKOH/gであることが好ましい。酸価が５０mgKOH/g未満の場合、アルカリ水溶液に対する溶解性が不十分で現像不良を生じやすく、一方、２５０mgKOH/gを超えた場合、現像時に塗膜の密着性の劣化や光硬化部（露光部）の溶解が生じてしまう。 Moreover, it is preferable that the acid value of the organic binder used is 50-250 mgKOH / g. When the acid value is less than 50 mgKOH / g, the solubility in an alkaline aqueous solution is insufficient, and development failure tends to occur. On the other hand, when the acid value exceeds 250 mgKOH / g, the adhesion of the coating film is deteriorated during development or the photocured part (exposure). Part) will be dissolved.
さらに、カルボキシル基含有感光性樹脂の二重結合当量が、３５０〜２，０００g/eqであることが好ましい。カルボキシル基含有感光性樹脂の二重結合当量が３５０g/eq未満の場合、パターンが太りやすく、ラインのシャープ性が悪化しやすい。一方、２，０００g/eqを超えた場合、現像時の作業余裕度が狭く、また光硬化時に高露光量を必要とする。より好ましくは４００〜１，５００g/eqである。 Further, the double bond equivalent of the carboxyl group-containing photosensitive resin is preferably 350 to 2,000 g / eq. When the double bond equivalent of the carboxyl group-containing photosensitive resin is less than 350 g / eq, the pattern tends to be thick and the line sharpness tends to deteriorate. On the other hand, if it exceeds 2,000 g / eq, the work margin during development is narrow, and a high exposure amount is required during photocuring. More preferably, it is 400-1500 g / eq.
光重合性モノマーとしては、例えば２−ヒドロキシエチルアクリレート、２−ヒドロキシプロピルアクリレート、ジエチレングリコールジアクリレート、トリエチレングリコールジアクリレート、ポリエチレングリコールジアクリレート、ポリウレタンジアクリレート、トリメチロールプロパントリアクリレート、ペンタエリスリトールトリアクリレート、ペンタエリスリトールテトラアクリレート、トリメチロールプロパンエチレンオキサイド変性トリアクリレート、ジペンタエリスリトールペンタアクリレート、ジペンタエリスリトールヘキサアクリレートおよび上記アクリレートに対応する各メタクリレート類；フタル酸、アジピン酸、マレイン酸、イタコン酸、コハク酸、トリメリット酸、テレフタル酸などの多塩基酸とヒドロキシアルキル（メタ）アクリレートとのモノ−、ジ−、トリ−、またはそれ以上のポリエステルなどが挙げられる。 Examples of the photopolymerizable monomer include 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, diethylene glycol diacrylate, triethylene glycol diacrylate, polyethylene glycol diacrylate, polyurethane diacrylate, trimethylolpropane triacrylate, pentaerythritol triacrylate, Pentaerythritol tetraacrylate, trimethylolpropane ethylene oxide modified triacrylate, dipentaerythritol pentaacrylate, dipentaerythritol hexaacrylate and the corresponding methacrylates; phthalic acid, adipic acid, maleic acid, itaconic acid, succinic acid, Polybasic acids such as trimellitic acid and terephthalic acid and hydroxy Alkyl (meth) mono acrylate -, di -, tri -, or the like more polyesters.
これら光重合性モノマーは、単独でまたは２種以上を組み合わせて用いることができる。また、これらの光重合性モノマーの中でも、１分子中に２個以上のアクリロイル基またはメタクリロイル基を有する多官能モノマーが好ましい。 These photopolymerizable monomers can be used alone or in combination of two or more. Among these photopolymerizable monomers, polyfunctional monomers having two or more acryloyl groups or methacryloyl groups in one molecule are preferable.
このような光重合性モノマーの配合量としては、固形分換算として、有機バインダー１００質量部あたり５〜２００質量部が好ましい。 As a compounding quantity of such a photopolymerizable monomer, 5-200 mass parts is preferable per 100 mass parts of organic binders as solid content conversion.
本実施形態の感光性導電ペーストにおける導電性粉末は、形成された導電回路に導電性を付与するものであり、具体的には、例えばAg、Au、Pt、Pd、Ni、Cu、Al、Sn、Pb、Zn、Fe、Ir、Os、Rh、W、Mo、Ruなどを挙げることができる。これらの導電性粉末は、単体の形態で用いてもよいし、これらのいずれかの合金や、これらのいずれかをコアまたは被覆層とする多層体であってもよい。また、酸化錫（SnO2）、酸化インジウム（In2O3）、ITO（Indium Tin Oxide）などの酸化物を用いてもよい。これら導電性粉末の中でもAgが好適に用いられる。 The conductive powder in the photosensitive conductive paste of the present embodiment imparts conductivity to the formed conductive circuit. Specifically, for example, Ag, Au, Pt, Pd, Ni, Cu, Al, Sn , Pb, Zn, Fe, Ir, Os, Rh, W, Mo, Ru, and the like. These conductive powders may be used in the form of a single body, or may be any of these alloys, or a multilayer body having any of these as a core or a coating layer. Further, oxides such as tin oxide (SnO 2 ), indium oxide (In 2 O 3 ), and ITO (Indium Tin Oxide) may be used. Among these conductive powders, Ag is preferably used.
導電性粉末の形状としては、球状、フレーク（鱗片）状の他、デントライト状など種々の形状のものを用いることができ、特に限定されない。 The shape of the conductive powder is not particularly limited, and may be various shapes such as a dentlite shape as well as a spherical shape and a flake shape.
導電性粉末の粒径としては、特に制限はないが、例えば球状の導電性粉末を用いる場合は、平均粒径が０．１〜５μｍ、好ましくは０．２〜３μｍである。また、フレーク状の導電性粉末を用いる場合、平均粒径が０．１〜５μｍ、好ましくは０．３〜３μｍである。
なお、平均粒径は、ＳＥＭ（走査型電子顕微鏡）を用いて観察したランダムな１０個の導電性粉末を測定した平均を算出することで求められる。
また、フレーク状銀粉末とは、具体的にはアスペクト比が３以上である銀粉をいう。アスペクト比は、（平均粒径／平均厚さＴ）により求めることができる。
ここで、「平均粒径」は、走査型電子顕微鏡で長手方向に測定した粒子１０個の平均長径Ｌを示し、「平均厚さＴ」は、走査型電子顕微鏡で厚さ方向に測定した粒子１０個の平均厚さＴを示す。
Although there is no restriction | limiting in particular as a particle size of electroconductive powder, For example, when using spherical electroconductive powder, an average particle diameter is 0.1-5 micrometers, Preferably it is 0.2-3 micrometers. Moreover, when using flaky conductive powder, an average particle diameter is 0.1-5 micrometers, Preferably it is 0.3-3 micrometers.
In addition, an average particle diameter is calculated | required by calculating the average which measured 10 random electroconductive powders observed using SEM (scanning electron microscope).
The flaky silver powder specifically refers to silver powder having an aspect ratio of 3 or more. The aspect ratio can be obtained by (average particle diameter / average thickness T).
Here, “average particle diameter” indicates an average long diameter L of 10 particles measured in the longitudinal direction with a scanning electron microscope, and “average thickness T” indicates particles measured in the thickness direction with a scanning electron microscope. Ten average thicknesses T are shown.
このような導電性粉末は、感光性導電ペーストの不揮発成分（乾燥工程でペースト中から揮発せず、膜に残存する成分）を基準として、３０〜９０質量％であることが好ましい。３０質量％未満であると、十分な導電性を得ることが困難となり、９０質量％を超えると、露光時の光が塗膜深部まで透過しないため、深部の光硬化性が悪くなり、細線パターンの形成が出来なくなる。より好ましくは５０〜８５質量％である。 Such conductive powder is preferably 30 to 90% by mass based on the nonvolatile component of the photosensitive conductive paste (the component that does not volatilize from the paste in the drying step and remains in the film). If it is less than 30% by mass, it will be difficult to obtain sufficient electrical conductivity. If it exceeds 90% by mass, the light at the time of exposure will not penetrate to the deep part of the coating film, so that the photocurability of the deep part will deteriorate, and the fine line pattern Cannot be formed. More preferably, it is 50-85 mass%.
チオジグリコール酸は、従来金属めっき液の安定性の付与のため添加させるものであるが、本実施形態においては、上記のとおり導電回路形成に用いる感光性導電ペーストとして後述のオキシムエステル系光重合開始剤と併用することで高解像、且つ低抵抗の導電回路形成を達成することができる。
関東化学社製の鹿１級等のチオジグリコール酸を使用することができる。
また、チオジグリコール酸の誘導体を用いても低抵抗の導電回路の形成を達成することができる。
チオジグリコール酸の誘導体としては、例えば３，３’−チオジプロピオン酸、チオ二酢酸ジアリル、チオビス（酢酸ブチル）、チオジグリコール酸ジナトリウム、２，２’−チオ二酢酸ビス（２−エチルヘキシル）、チオ二酢酸ジオクチル、２，２’−チオビス（酢酸メチル）、チオジグリコール酸ジカリウム等があげられる。
Thiodiglycolic acid is conventionally added to impart stability of the metal plating solution, but in this embodiment, as described above, the oxime ester-based photopolymerization described later as the photosensitive conductive paste used for forming the conductive circuit as described above. By using it together with an initiator, it is possible to achieve high resolution and low resistance conductive circuit formation.
A thiodiglycolic acid such as deer grade 1 manufactured by Kanto Chemical Co., Inc. can be used.
In addition, formation of a low-resistance conductive circuit can be achieved using a thiodiglycolic acid derivative.
Examples of thiodiglycolic acid derivatives include 3,3′-thiodipropionic acid, diallyl thiodiacetic acid, thiobis (butyl acetate), disodium thiodiglycolate, bis (2,2′-thiodiacetic acid bis (2- Ethylhexyl), dioctyl thiodiacetate, 2,2′-thiobis (methyl acetate), dipotassium thiodiglycolate and the like.
チオジグリコール酸およびチオジグリコール酸の誘導体の少なくとも何れか１種の配合割合は、固形分換算として、有機バインダー１００質量部あたり０．０１〜１０質量部が好ましい。０．０１質量部未満であると、導電性が悪化してしまうため、好ましくない。一方、１０質量部を超えると、同様に導電性が悪化してしまい、また、現像性が非常に良いチオジグリコール酸およびチオジグリコール酸の誘導体の少なくとも何れか１種の特性により、パターング性が悪化するため、好ましくない。より好ましくは、０．１〜５質量部である。 The blending ratio of at least one of thiodiglycolic acid and thiodiglycolic acid derivatives is preferably 0.01 to 10 parts by mass per 100 parts by mass of the organic binder in terms of solid content. If it is less than 0.01 parts by mass, the conductivity is deteriorated, which is not preferable. On the other hand, when the amount exceeds 10 parts by mass, the conductivity deteriorates in the same manner, and the patterning property is improved by at least one of the properties of thiodiglycolic acid and thiodiglycolic acid derivatives having very good developability. Is not preferable because it deteriorates. More preferably, it is 0.1-5 mass parts.
オキシムエステル系光重合開始剤は、高光感度であるため導電性粉末が多く配合されたペーストであっても、少ない露光量で十分に光硬化を行うことができ、解像性の高い導電回路を形成することができる。
このようなオキシムエステル系光重合開始剤としては、例えば下記一般式（I）で表わされる基を有する化合物、
下記一般式（II）で示される２−（アセチルオキシイミノメチル）チオキサンテン−９−オン、
下記一般式（IV）で表される化合物、
下記一般式（V）で表される化合物や、
下記一般式（VI）で表されるカルバゾール２量体を有する化合物を用いることができる。
As such an oxime ester photopolymerization initiator, for example, a compound having a group represented by the following general formula (I),
2- (acetyloxyiminomethyl) thioxanthen-9-one represented by the following general formula (II):
A compound represented by the following general formula (IV):
A compound represented by the following general formula (V),
A compound having a carbazole dimer represented by the following general formula (VI) can be used.
市販品としては、例えばBASFジャパン社製のCGI-325、IRGACURE（登録商標）OXE01、IRGACURE OXE02、ADEKA社製のNCI-831などを用いることができる。 Examples of commercially available products include CGI-325 manufactured by BASF Japan, IRGACURE (registered trademark) OXE01, IRGACURE OXE02, NCI-831 manufactured by ADEKA, and the like.
オキシムエステル系光重合開始剤の配合割合は、固形分換算として、有機バインダー１００質量部あたり０．０１〜３０質量部が好ましい。０．０１質量部未満であると、光硬化性が不十分になりパターンに欠けが発生しやすくなる。また表面硬化性が不足し、現像時に塗膜表面がダメージを受け、抵抗値の悪化が起きる。 一方、３０質量部を超えると、パターンのハレーションが発生し、パターンエッジ部分のシャープ性が悪化する。またパターンのぬき性が悪化し、スペースが小さいパターンが描けなくなる。より好ましくは、０．０５〜５質量部である。 The blending ratio of the oxime ester-based photopolymerization initiator is preferably 0.01 to 30 parts by mass per 100 parts by mass of the organic binder in terms of solid content. If it is less than 0.01 parts by mass, the photocurability becomes insufficient and the pattern tends to be chipped. Further, the surface curability is insufficient, the coating surface is damaged during development, and the resistance value is deteriorated. On the other hand, if it exceeds 30 parts by mass, pattern halation occurs and the sharpness of the pattern edge portion deteriorates. In addition, the penetrability of the pattern deteriorates, and a pattern with a small space cannot be drawn. More preferably, it is 0.05-5 mass parts.
また、上記したオキシムエステル系以外の光重合開始剤を併用してもよい。このような光重合開始剤としては、具体例には、例えばベンゾイン、ベンゾインメチルエーテル、ベンゾインエチルエーテル、ベンゾインイソプロピルエーテルなどのベンゾインとベンゾインアルキルエーテル類；アセトフェノン、２，２−ジメトキシ−２−フェニルアセトフェノン、２，２−ジエトキシ−２−フェニルアセトフェノン、１，１−ジクロロアセトフェノンなどのアセトフェノン類；２−メチル−１−［４−（メチルチオ）フェニル］−２−モリフォリノプロパン−１−オン、２−ベンジル−２−ジメチルアミノ−１−（４−モリフォリノフェニル）−ブタノン−１、２−（ジメチルアミノ）−２−［（４−メチルフェニル）メチル］−１−［４−（４−モルホリニル）フェニル］−１−ブタノンなどのアミノアセトフェノン類；２−メチルアントラキノン、２−エチルアントラキノン、２−ｔ−ブチルアントラキノン、１−クロロアントラキノンなどのアントラキノン類；２，４−ジメチルチオキサントン、２，４−ジエチルチオキサントン、２−クロロチオキサントン、２，４−ジイソプロピルチオキサントンなどのチオキサントン類；アセトフェノンジメチルケタール、ベンジルジメチルケタールなどのケタール類；ベンゾフェノンなどのベンゾフェノン類；またはキサントン類；（２，６−ジメトキシベンゾイル）−２，４，４−ペンチルホスフィンオキサイド、ビス（２，４，６−トリメチルベンゾイル）−フェニルホスフィンオキサイド、２，４，６−トリメチルベンゾイルジフェニルホスフィンオキサイド、エチル−２，４，６−トリメチルベンゾイルジフェニルホスフィネートなどのホスフィンオキサイド類；各種パーオキサイド類が挙げられる。また、光重合開始剤としてはBASFジャパン社製のイルガキュア389も好適に用いることが出来る。 Moreover, you may use together photoinitiators other than the above-mentioned oxime ester type | system | group. Specific examples of such photopolymerization initiators include benzoin and benzoin alkyl ethers such as benzoin, benzoin methyl ether, benzoin ethyl ether, and benzoin isopropyl ether; acetophenone, 2,2-dimethoxy-2-phenylacetophenone , Acetophenones such as 2,2-diethoxy-2-phenylacetophenone and 1,1-dichloroacetophenone; 2-methyl-1- [4- (methylthio) phenyl] -2-morpholinopropan-1-one, 2 -Benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butanone-1,2- (dimethylamino) -2-[(4-methylphenyl) methyl] -1- [4- (4- Aminoacetophenone such as morpholinyl) phenyl] -1-butanone Anthraquinones such as 2-methylanthraquinone, 2-ethylanthraquinone, 2-t-butylanthraquinone, 1-chloroanthraquinone; 2,4-dimethylthioxanthone, 2,4-diethylthioxanthone, 2-chlorothioxanthone, 2,4- Thioxanthones such as diisopropylthioxanthone; ketals such as acetophenone dimethyl ketal and benzyl dimethyl ketal; benzophenones such as benzophenone; or xanthones; (2,6-dimethoxybenzoyl) -2,4,4-pentylphosphine oxide, bis ( 2,4,6-trimethylbenzoyl) -phenylphosphine oxide, 2,4,6-trimethylbenzoyldiphenylphosphine oxide, ethyl-2,4,6-trimethylbenzoy Phosphine oxides such as diphenyl phosphinate; various peroxides and the like. As a photopolymerization initiator, Irgacure 389 manufactured by BASF Japan can also be suitably used.
市販品としては、例えばBASFジャパン社製のIRGACURE 184、IRGACURE 819、IRGACURE 907、IRGACURE 369、IRGACURE 379、ルシリン（登録商標）TPOなどが挙げられる。なお、これらに限定されるものではなく、また、これらの光重合開始剤を単独でまたは２種以上をオキシムエステル系光重合開始剤と組み合わせて用いることができる。 Examples of commercially available products include IRGACURE 184, IRGACURE 819, IRGACURE 907, IRGACURE 369, IRGACURE 379, and Lucillin (registered trademark) TPO manufactured by BASF Japan. In addition, it is not limited to these, Moreover, these photoinitiators can be used individually or in combination of 2 or more types with an oxime ester system photoinitiator.
また、上記した光重合開始剤は、Ｎ，Ｎ−ジメチルアミノ安息香酸エチルエステル、Ｎ，Ｎ−ジメチルアミノ安息香酸イソアミルエステル、ペンチル−４−ジメチルアミノベンゾエート、トリエチルアミン、トリエタノールアミンなどの三級アミン類のような光増感剤の1種あるいは2種以上と組み合わせて用いることができる。 The above-mentioned photopolymerization initiator includes tertiary amines such as N, N-dimethylaminobenzoic acid ethyl ester, N, N-dimethylaminobenzoic acid isoamyl ester, pentyl-4-dimethylaminobenzoate, triethylamine, and triethanolamine. It can be used in combination with one or more photosensitizers such as
また、必要に応じて未硬化の光重合性成分を反応させるために、熱重合触媒を上記した光重合開始剤と併用することができる。熱重合触媒は、数分から1時間程度の高温におけるエージングにより、未硬化の光重合性成分を反応させることができる。 Moreover, in order to react an uncured photopolymerizable component as needed, a thermal polymerization catalyst can be used in combination with the above-described photopolymerization initiator. The thermal polymerization catalyst can react with an uncured photopolymerizable component by aging at a high temperature of about several minutes to 1 hour.
このような熱重合触媒としては、例えば過酸化ベンゾイルなどの過酸化物、イソブチロニトリルなどのアゾ化合物であり、好ましくは、２，２’−アゾビスイソブチロニトリル、２，２’−アゾビス−２−メチルブチロニトリル、２，２’−アゾビス−２，４−ジバレロニトリル、１，１’−アゾビス−１−シクロヘキサンカルボニトリル、ジメチル−２，２’−アゾビスイソブチレイト、４，４’−アゾビス−４−シアノバレリックアシッド、２−メチル−２，２’−アゾビスプロパンニトリル、２，４−ジメチル−２，２，２’，２’−アゾビスペンタンニトリル、１，１’−アゾビス（１−アセトキシ−１−フェニルエタン）、２，２，２’，２’−アゾビス（２−メチルブタナミドオキシム）ジヒドロクロライドなどが挙げられる。 Examples of such a thermal polymerization catalyst include peroxides such as benzoyl peroxide and azo compounds such as isobutyronitrile, and preferably 2,2′-azobisisobutyronitrile, 2,2′- Azobis-2-methylbutyronitrile, 2,2′-azobis-2,4-divaleronitrile, 1,1′-azobis-1-cyclohexanecarbonitrile, dimethyl-2,2′-azobisisobutyrate, 4,4′-azobis-4-cyanovaleric acid, 2-methyl-2,2′-azobispropanenitrile, 2,4-dimethyl-2,2,2 ′, 2′-azobispentanenitrile, 1 , 1′-azobis (1-acetoxy-1-phenylethane), 2,2,2 ′, 2′-azobis (2-methylbutanamide oxime) dihydrochloride, and the like.
本実施態様の感光性導電ペーストには、粘度を調整し、均一な塗膜を形成するために有機溶剤を用いることができる。
このような有機溶剤としては、例えばメチルエチルケトン、シクロヘキサノンなどのケトン類；トルエン、キシレン、テトラメチルベンゼンなどの芳香族炭化水素類；セロソルブ、メチルセロソルブ、カルビトール、メチルカルビトール、ブチルカルビトール、プロピレングリコールモノメチルエーテル、ジプロピレングリコールモノメチルエーテル、ジプロピレングリコールモノエチルエーテル、トリエチレングリコールモノエチルエーテルなどのグリコールエーテル類；酢酸エチル、酢酸ブチル、セロソルブアセテート、ブチルセロソルブアセテート、カルビトールアセテート、ブチルカルビトールアセテート、プロピレングリコールモノメチルエーテルアセテート、２，２，４−トリメチル−１，３−ペンタンジオールモノイソブチレートなどのエステル類；エタノール、プロパノール、エチレングリコール、プロピレングリコール、テルピネオールなどのアルコール類；オクタン、デカンなどの脂肪族炭化水素；石油エーテル、石油ナフサ、水添石油ナフサ、ソルベントナフサなどの石油系溶剤が挙げられ、これらを単独でまたは２種以上を組み合わせて用いることができる。
In the photosensitive conductive paste of this embodiment, an organic solvent can be used in order to adjust the viscosity and form a uniform coating film.
Examples of such organic solvents include ketones such as methyl ethyl ketone and cyclohexanone; aromatic hydrocarbons such as toluene, xylene, and tetramethylbenzene; cellosolve, methyl cellosolve, carbitol, methyl carbitol, butyl carbitol, propylene glycol Glycol ethers such as monomethyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, triethylene glycol monoethyl ether; ethyl acetate, butyl acetate, cellosolve acetate, butyl cellosolve acetate, carbitol acetate, butyl carbitol acetate, propylene Glycol monomethyl ether acetate, 2,2,4-trimethyl-1,3-pentanediol monoisobutyle Esters such as ethanol; alcohols such as ethanol, propanol, ethylene glycol, propylene glycol, and terpineol; aliphatic hydrocarbons such as octane and decane; petroleum solvents such as petroleum ether, petroleum naphtha, hydrogenated petroleum naphtha, and solvent naphtha These can be used alone or in combination of two or more.
このような感光性導電ペーストにおいて、さらに、保存安定性を向上させ、ゲル化や流動性の低下による塗布作業性の悪化を抑制するために、安定剤を添加することができる。 In such a photosensitive conductive paste, a stabilizer can be added in order to further improve the storage stability and suppress the deterioration of the coating workability due to the gelation or the decrease in fluidity.
このような安定剤としては、感光性導電ペースト中の導電性粉末との錯体化あるいは塩形成などの効果のある化合物を用いることができる。 As such a stabilizer, a compound having an effect of complexing with the conductive powder in the photosensitive conductive paste or forming a salt can be used.
具体的には、例えば硝酸、硫酸、塩酸、ホウ酸などの各種無機酸；ギ酸、酢酸、アセト酢酸、クエン酸、ステアリン酸、マレイン酸、フマル酸、フタル酸、ベンゼンスルホン酸、スルファミン酸などの各種有機酸；リン酸、亜リン酸、次亜リン酸、リン酸メチル、リン酸エチル、リン酸ブチル、リン酸フェニル、亜リン酸エチル、亜リン酸ジフェニル、モノ（２−メタクリロイルオキシエチル）アシッドホスフェート、ジ（２−メタクリロイルオキシエチル）アシッドホスフェートなどの各種リン酸化合物（無機リン酸、有機リン酸）などの酸が挙げられる。これら安定剤は単独でまたは２種以上を組み合わせて用いることができる。 Specifically, for example, various inorganic acids such as nitric acid, sulfuric acid, hydrochloric acid, boric acid; formic acid, acetic acid, acetoacetic acid, citric acid, stearic acid, maleic acid, fumaric acid, phthalic acid, benzenesulfonic acid, sulfamic acid, etc. Various organic acids; phosphoric acid, phosphorous acid, hypophosphorous acid, methyl phosphate, ethyl phosphate, butyl phosphate, phenyl phosphate, ethyl phosphite, diphenyl phosphite, mono (2-methacryloyloxyethyl) Examples include acids such as various phosphate compounds (inorganic phosphoric acid, organic phosphoric acid) such as acid phosphate and di (2-methacryloyloxyethyl) acid phosphate. These stabilizers can be used alone or in combination of two or more.
さらに、本実施形態の感光性導電ペーストには、シリコーン系、アクリル系などの消泡・レベリング剤、塗膜の密着性向上のためのシランカップリング剤などの他の添加剤を配合することができる。またさらに、公知の酸化防止剤や保存時の熱的安定性を向上させるための熱重合禁止剤などを添加することもできる。 Furthermore, the photosensitive conductive paste of the present embodiment may be blended with other additives such as a defoaming / leveling agent such as silicone and acrylic, and a silane coupling agent for improving the adhesion of the coating film. it can. Furthermore, a known antioxidant or a thermal polymerization inhibitor for improving the thermal stability during storage may be added.
以上のように構成される感光性導電ペーストは、各成分を混合することにより調製され、攪拌機等による攪拌の後、３本ロールミルなどにより練肉してペースト化することができる。 The photosensitive electrically conductive paste comprised as mentioned above is prepared by mixing each component, and after stirring with a stirrer etc., it can knead | mix with a 3 roll mill etc. and can be made into a paste.
このようにして調製された感光性導電ペーストは、スクリーン印刷法、バーコーダー、ブレードコーターなど適宜の塗布方法で、ガラス基板などの基材に塗布し、塗膜を形成する。 The photosensitive conductive paste thus prepared is applied to a substrate such as a glass substrate by an appropriate application method such as a screen printing method, a bar coder, or a blade coater to form a coating film.
次いで、得られた塗膜を、指触乾燥性を得るために熱風循環式乾燥炉、遠赤外線乾燥炉などで例えば約７０〜１２０℃で５〜４０分程度乾燥させ、タックフリーの塗膜（乾燥塗膜）を形成する。このとき、予め感光性導電ペーストをフィルム上に成膜している場合には、基材上にラミネートしてもよい。 Next, the obtained coating film is dried at, for example, about 70 to 120 ° C. for about 5 to 40 minutes in a hot-air circulating drying furnace, a far-infrared drying furnace or the like in order to obtain a touch-drying property. Dry film). At this time, when a photosensitive conductive paste is previously formed on a film, it may be laminated on a substrate.
その後、得られた乾燥塗膜に対し、選択的露光を行う。選択的露光としては、所定の露光パターンを有するネガマスクを用いた接触露光および非接触露光が可能である。露光光源としては、例えばハロゲンランプ、高圧水銀灯、レーザー光、メタルハライドランプ、ブラックランプ、無電極ランプなどが使用される。露光量としては１０〜７００mJ/cm2程度が好ましい。 Then, selective exposure is performed with respect to the obtained dry coating film. As selective exposure, contact exposure and non-contact exposure using a negative mask having a predetermined exposure pattern are possible. As the exposure light source, for example, a halogen lamp, a high-pressure mercury lamp, a laser beam, a metal halide lamp, a black lamp, an electrodeless lamp, or the like is used. The exposure dose is preferably about 10 to 700 mJ / cm 2 .
選択的露光後の塗膜に対し、現像を行う。現像にはスプレー法、浸漬法などが用いられる。現像液としては、感光性導電ペースト中に含まれるカルボキシル基含有樹脂のカルボキシル基がケン化され、未硬化部（未露光部）を除去することができればよく、例えば、水酸化ナトリウム、水酸化カリウム、炭酸ナトリウム、炭酸カリウム、珪酸ナトリウム等の金属アルカリ水溶液や、モノエタノールアミン、ジエタノールアミン、トリエタノールアミン等のアミン水溶液、特に約1.5wt％以下の濃度の希アルカリ水溶液が好適に用いられる。また、現像後に不要な現像液の除去のため、水洗や酸中和を行うことが好ましい。 Development is performed on the coating film after selective exposure. For the development, a spray method, a dipping method or the like is used. As the developer, it is sufficient that the carboxyl group of the carboxyl group-containing resin contained in the photosensitive conductive paste is saponified and the uncured part (unexposed part) can be removed. For example, sodium hydroxide, potassium hydroxide Metal alkali aqueous solutions such as sodium carbonate, potassium carbonate, and sodium silicate, amine aqueous solutions such as monoethanolamine, diethanolamine, and triethanolamine, particularly dilute alkaline aqueous solutions having a concentration of about 1.5 wt% or less are preferably used. Moreover, it is preferable to perform washing with water and acid neutralization in order to remove an unnecessary developer after development.
その後、現像により所望の回路パターンが形成された基板を、８０〜３００℃で５〜６０分乾燥、または硬化させることで基材上に所望の導電回路を形成する。 Thereafter, the substrate on which the desired circuit pattern is formed by development is dried or cured at 80 to 300 ° C. for 5 to 60 minutes to form a desired conductive circuit on the base material.
以下、実施例および比較例を示して本実施形態について具体的に説明するが、本発明は、これら実施例に限定されるものではない。尚、以下において「%」とあるのは、特に断りのない限り全て重量基準である。 Hereinafter, although an Example and a comparative example are shown and this embodiment is demonstrated concretely, this invention is not limited to these Examples. In the following, “%” is based on weight unless otherwise specified.
〈有機バインダーの合成例〉
温度計、攪拌機、滴下ロート、および還流冷却器を備えたフラスコに、メチルメタクリレート、メタクリル酸を０．８７：０．１３のモル比で仕込み、溶媒としてジプロピレングリコールモノメチルエーテル、触媒としてアゾビスイソブチロ二トリルを入れ、窒素雰囲気下、８０℃で２〜６時間攪拌し、有機バインダーを含む樹脂溶液を得た。この有機バインダーは、重量平均分子量が約１０，０００、酸価が７４mgKOH/g、固形分が５７％であった。
<Synthesis example of organic binder>
A flask equipped with a thermometer, stirrer, dropping funnel, and reflux condenser is charged with methyl methacrylate and methacrylic acid in a molar ratio of 0.87: 0.13, dipropylene glycol monomethyl ether as a solvent, and azobisiso as a catalyst. Butyronitryl was added and stirred at 80 ° C. for 2 to 6 hours under a nitrogen atmosphere to obtain a resin solution containing an organic binder. This organic binder had a weight average molecular weight of about 10,000, an acid value of 74 mgKOH / g, and a solid content of 57%.
得られた有機バインダーの重量平均分子量の測定には、島津製作所製ポンプＬＣ−６ＡＤと昭和電工製カラムＳｈｏｄｅｘ(登録商標)ＫＦ−８０４、ＫＦ−８０３、ＫＦ−８０２を３本つないだ高速液体クロマトグラフィーを使用した。 For the measurement of the weight average molecular weight of the obtained organic binder, a high performance liquid chromatograph in which three pumps LC-6AD manufactured by Shimadzu Corporation and three columns Shodex (registered trademark) KF-804, KF-803, and KF-802 manufactured by Showa Denko were connected. The graphic was used.
（感光性導電ペーストの調製）
表１に示す各成分・組成比にて配合し、攪拌機により攪拌後、３本ロールミルにより練肉してペースト化を行い、実施例１、２および比較例１、２の各感光性導電ペーストを調製した。なお、感光性導電ペーストに用いる導電性粉末の明度L*値は、JIS規格Z8722に従い測定した値である。
(Preparation of photosensitive conductive paste)
It mixes with each component and composition ratio shown in Table 1, and after stirring with a stirrer, it pastes by kneading with a 3 roll mill, and each photosensitive conductive paste of Examples 1, 2 and Comparative Examples 1, 2 is used. Prepared. The lightness L * value of the conductive powder used for the photosensitive conductive paste is a value measured according to JIS standard Z8722.
＊１：明度L*=７０、平均粒径＝２μｍ
＊２：明度L*= ５８、平均粒径＝１．５μｍ
＊３：オキシムエステル系光重合開始剤；IRGACURE OXE02（BASFジャパン社製）
＊４：チオキサントン系光重合開始剤；KAYACURE DETX-S（日本化薬社製）
＊５：アセトアミノフェノン系重合開始剤；IRGACURE 379（BASFジャパン社製）
＊６：２,２’−チオジグリコール酸（関東化学社製；規格 鹿１級）
＊７：Ｍ−３５０（東亞合成社製）
＊８：カルビトールアセテート
＊９：ＢＹＫ−３５４（ビックケミー・ジャパン社製）
＊１０：不揮発成分を基準として算出。
* 1: Lightness L * = 70, average particle size = 2 μm
* 2: Lightness L * = 58, average particle size = 1.5 μm
* 3: Oxime ester photoinitiator; IRGACURE OXE02 (BASF Japan)
* 4: Thioxanthone photopolymerization initiator; KAYACURE DETX-S (Nippon Kayaku Co., Ltd.)
* 5: Acetaminophenone polymerization initiator; IRGACURE 379 (BASF Japan)
* 6: 2,2′-thiodiglycolic acid (manufactured by Kanto Chemical Co., Inc .; standard deer grade 1)
* 7: M-350 (Toagosei Co., Ltd.)
* 8: Carbitol acetate * 9: BYK-354 (by Big Chemie Japan)
* 10: Calculated based on nonvolatile components.
〈評価用回路の作成〉
ガラス基板上に、各感光性導電ペーストを、２００メッシュのポリエステルスクリーンを用いて、ウェット膜厚が１４μｍとなるように全面に塗布し、IR乾燥炉にて、１００℃で２０分間乾燥して、乾燥塗膜を形成した。なお、乾燥後の塗膜の膜厚は１０μｍであった。
<Creation of evaluation circuit>
Each photosensitive conductive paste was applied on the entire surface of the glass substrate using a 200 mesh polyester screen so that the wet film thickness was 14 μm, and dried at 100 ° C. for 20 minutes in an IR drying furnace. A dry coating was formed. In addition, the film thickness of the coating film after drying was 10 μm.
次に、得られた乾燥塗膜に、光源として超高圧水銀灯を用い、ネガマスクを介して、残し解像度はライン＝１０／２０／〜９０／１００μｍのストレートラインパターンネガマスクを使用した。抜き解像度については残し解像度のネガパターンのネガ／ポジ逆パターンを使用した。各パターン露光した後、液温３０℃の０．４％炭酸ナトリウム水溶液を用いて現像時間を１０および２０秒として現像を行い、水洗した。 Next, an ultrahigh pressure mercury lamp was used as a light source for the obtained dried coating film, and a straight line pattern negative mask having a remaining resolution of 10 = 20/90 to 100/100 μm was used through a negative mask. For the blanking resolution, a negative / positive reverse pattern of the negative resolution of the remaining resolution was used. After each pattern exposure, development was performed using a 0.4% sodium carbonate aqueous solution with a liquid temperature of 30 ° C. for a development time of 10 and 20 seconds, followed by washing with water.
（回路形成性評価）
残し解像度；最小残存パターンのネガマスク設計値。
抜き解像度；パターニングが出来た最小スペースのネガマスク設計値。
測定結果を表２に示す。
(Circuit formability evaluation)
Remaining resolution: negative mask design value of the minimum remaining pattern.
Extraction resolution: Negative mask design value of the smallest space that can be patterned.
The measurement results are shown in Table 2.
（比抵抗値評価）
ネガ設計０．４×１０（ｃｍ）の長方形パターンを形成し、熱硬化後の抵抗値と膜厚から比抵抗値を算出した。測定結果を表２に示す。
(Specific resistance evaluation)
A rectangular pattern having a negative design of 0.4 × 10 (cm) was formed, and the specific resistance value was calculated from the resistance value and the film thickness after thermosetting. The measurement results are shown in Table 2.
表２に示すように、本実施形態の感光性導電ペーストを用いた実施例１、２とも銀粉によらず残し解像度、抜き解像度が良く、低抵抗であることが分かる。また、実施例１、２の結果より本実施形態の感光性導電ペーストにおいて、導電性粉末の明度L*値に関わらずパターニングは良好であることが分かる。
一方、光重合開始剤にオキシムエステル系を使用しなかった比較例１では光硬化が不十分で残し解像度の低下が確認された。また塗膜表面の光硬化が不十分なため現像のダメージを受け比抵抗値の悪化が確認された。また、チオジグリコール酸およびチオジグリコール酸の誘導体の少なくとも何れか１種を使用しなかった比較例２では、抵抗値が悪化することがわかる。
As shown in Table 2, it can be seen that both Examples 1 and 2 using the photosensitive conductive paste of the present embodiment have good resolution and removal resolution regardless of silver powder, and have low resistance. Further, it can be seen from the results of Examples 1 and 2 that the patterning is good in the photosensitive conductive paste of this embodiment regardless of the lightness L * value of the conductive powder.
On the other hand, in Comparative Example 1 in which no oxime ester was used as the photopolymerization initiator, photocuring was insufficient and the resolution was lowered. Moreover, since the photocuring of the coating film surface was insufficient, the development resistance was damaged, and the specific resistance value was confirmed to deteriorate. Moreover, it turns out that resistance value deteriorates in the comparative example 2 which did not use at least any 1 type of the derivative of thiodiglycolic acid and thiodiglycolic acid.
Claims (3)
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| JP2012080921A JP5916482B2 (en) | 2012-03-30 | 2012-03-30 | Photosensitive conductive paste and conductive circuit |
| TW102107839A TWI550643B (en) | 2012-03-30 | 2013-03-06 | Conductive paste and conductive circuit |
| CN201310084011.8A CN103366861B (en) | 2012-03-30 | 2013-03-15 | Conductive paste and conducting channel |
| KR1020130029000A KR101568056B1 (en) | 2012-03-30 | 2013-03-19 | Conductive paste and conductive circuit |
| KR20150004366A KR20150022936A (en) | 2012-03-30 | 2015-01-12 | Conductive paste and conductive circuit |
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| JP4886444B2 (en) * | 2005-10-07 | 2012-02-29 | 石原産業株式会社 | Fluid composition, electrode formed using the same, wiring pattern, coating film, and decorative article formed with the coating film |
| US7655864B2 (en) * | 2006-07-13 | 2010-02-02 | E.I Du Pont De Nemours And Company | Photosensitive conductive paste for electrode formation and electrode |
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