JP5846829B2 - Photosensitive conductive paste - Google Patents
Photosensitive conductive paste Download PDFInfo
- Publication number
- JP5846829B2 JP5846829B2 JP2011216753A JP2011216753A JP5846829B2 JP 5846829 B2 JP5846829 B2 JP 5846829B2 JP 2011216753 A JP2011216753 A JP 2011216753A JP 2011216753 A JP2011216753 A JP 2011216753A JP 5846829 B2 JP5846829 B2 JP 5846829B2
- Authority
- JP
- Japan
- Prior art keywords
- group
- conductive paste
- acid
- silver powder
- pattern
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 42
- -1 oxime ester Chemical class 0.000 claims description 33
- 239000011347 resin Substances 0.000 claims description 28
- 229920005989 resin Polymers 0.000 claims description 28
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 23
- 239000011521 glass Substances 0.000 claims description 23
- 239000003999 initiator Substances 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 21
- 239000011230 binding agent Substances 0.000 claims description 14
- 239000000178 monomer Substances 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 10
- 125000004432 carbon atom Chemical group C* 0.000 description 38
- 125000000217 alkyl group Chemical group 0.000 description 33
- 239000010408 film Substances 0.000 description 23
- 239000011248 coating agent Substances 0.000 description 20
- 238000000576 coating method Methods 0.000 description 20
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 11
- 238000000034 method Methods 0.000 description 11
- 239000000758 substrate Substances 0.000 description 11
- 238000011161 development Methods 0.000 description 10
- 230000018109 developmental process Effects 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 10
- 238000010304 firing Methods 0.000 description 10
- 239000004020 conductor Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 125000003545 alkoxy group Chemical group 0.000 description 7
- 125000005843 halogen group Chemical group 0.000 description 7
- 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
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 6
- 125000004430 oxygen atom Chemical group O* 0.000 description 6
- 238000000016 photochemical curing Methods 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 150000007519 polyprotic acids Polymers 0.000 description 6
- 125000002252 acyl group Chemical group 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
- 239000002270 dispersing agent Substances 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000003381 stabilizer Substances 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 4
- 125000000753 cycloalkyl 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
- 238000002156 mixing Methods 0.000 description 4
- 239000000203 mixture 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
- 239000000049 pigment Substances 0.000 description 4
- 239000002904 solvent Substances 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
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 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
- 125000003282 alkyl amino group Chemical group 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 229960002130 benzoin Drugs 0.000 description 3
- 229920001400 block copolymer Polymers 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
- 125000004663 dialkyl amino group Chemical group 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 235000019382 gum benzoic Nutrition 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000012719 thermal polymerization Methods 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
- RBGUKBSLNOTVCD-UHFFFAOYSA-N 1-methylanthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2C RBGUKBSLNOTVCD-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
- 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
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-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
- 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 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
- 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
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 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
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- ALBJGICXDBJZGK-UHFFFAOYSA-N [1-[(1-acetyloxy-1-phenylethyl)diazenyl]-1-phenylethyl] acetate Chemical compound C=1C=CC=CC=1C(C)(OC(=O)C)N=NC(C)(OC(C)=O)C1=CC=CC=C1 ALBJGICXDBJZGK-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000012965 benzophenone Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- KVNRLNFWIYMESJ-UHFFFAOYSA-N butyronitrile Chemical compound CCCC#N KVNRLNFWIYMESJ-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 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
- 230000000694 effects Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 150000002576 ketones Chemical class 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
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 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
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 150000002894 organic compounds Chemical group 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
- 239000002685 polymerization catalyst Substances 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
- 238000002360 preparation method Methods 0.000 description 2
- 230000007261 regionalization Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- CNHDIAIOKMXOLK-UHFFFAOYSA-N toluquinol Chemical compound CC1=CC(O)=CC=C1O CNHDIAIOKMXOLK-UHFFFAOYSA-N 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
- 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
- DAFHKNAQFPVRKR-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylpropanoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)C DAFHKNAQFPVRKR-UHFFFAOYSA-N 0.000 description 1
- 125000004169 (C1-C6) alkyl group Chemical group 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
- 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
- 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
- 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
- BRKORVYTKKLNKX-UHFFFAOYSA-N 2,4-di(propan-2-yl)thioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(C(C)C)=CC(C(C)C)=C3SC2=C1 BRKORVYTKKLNKX-UHFFFAOYSA-N 0.000 description 1
- 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 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
- 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
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-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
- 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
- HEQOJEGTZCTHCF-UHFFFAOYSA-N 2-amino-1-phenylethanone Chemical class NCC(=O)C1=CC=CC=C1 HEQOJEGTZCTHCF-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
- MWDGNKGKLOBESZ-UHFFFAOYSA-N 2-oxooctanal Chemical compound CCCCCCC(=O)C=O MWDGNKGKLOBESZ-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
- ARXVXVOLXMVYIT-UHFFFAOYSA-N 3-methylbutyl 2-(dimethylamino)benzoate Chemical compound CC(C)CCOC(=O)C1=CC=CC=C1N(C)C ARXVXVOLXMVYIT-UHFFFAOYSA-N 0.000 description 1
- VFXXTYGQYWRHJP-UHFFFAOYSA-N 4,4'-azobis(4-cyanopentanoic acid) Chemical compound OC(=O)CCC(C)(C#N)N=NC(C)(CCC(O)=O)C#N VFXXTYGQYWRHJP-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 125000000590 4-methylphenyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)C([H])([H])[H] 0.000 description 1
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 1
- WDJHALXBUFZDSR-UHFFFAOYSA-N Acetoacetic acid Natural products CC(=O)CC(O)=O WDJHALXBUFZDSR-UHFFFAOYSA-N 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- 0 CC(C)(*)C(CC=C1)C=C1C(ON=C(*)C(c(c(*)c1*)c(*)c(*=C)c1NC1=CC=CC(C)(*)C=C1)=O)=O Chemical compound CC(C)(*)C(CC=C1)C=C1C(ON=C(*)C(c(c(*)c1*)c(*)c(*=C)c1NC1=CC=CC(C)(*)C=C1)=O)=O 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical group [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 description 1
- VMKBJESZDNXQHG-UHFFFAOYSA-N [(9-oxothioxanthen-2-yl)methylideneamino] acetate Chemical compound C1=CC=C2C(=O)C3=CC(C=NOC(=O)C)=CC=C3SC2=C1 VMKBJESZDNXQHG-UHFFFAOYSA-N 0.000 description 1
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 1
- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 description 1
- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 description 1
- KYIKRXIYLAGAKQ-UHFFFAOYSA-N abcn Chemical compound C1CCCCC1(C#N)N=NC1(C#N)CCCCC1 KYIKRXIYLAGAKQ-UHFFFAOYSA-N 0.000 description 1
- 150000008062 acetophenones Chemical class 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
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- 239000003513 alkali Substances 0.000 description 1
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- 150000001340 alkali metals Chemical class 0.000 description 1
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- 125000002947 alkylene group Chemical group 0.000 description 1
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
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- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
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- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
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- 125000004618 benzofuryl group Chemical group O1C(=CC2=C1C=CC=C2)* 0.000 description 1
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- 125000004196 benzothienyl group Chemical group S1C(=CC2=C1C=CC=C2)* 0.000 description 1
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- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 125000000609 carbazolyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3NC12)* 0.000 description 1
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- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
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- 238000013329 compounding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
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- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
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- WOWBFOBYOAGEEA-UHFFFAOYSA-N diafenthiuron Chemical compound CC(C)C1=C(NC(=S)NC(C)(C)C)C(C(C)C)=CC(OC=2C=CC=CC=2)=C1 WOWBFOBYOAGEEA-UHFFFAOYSA-N 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 1
- KUMNEOGIHFCNQW-UHFFFAOYSA-N diphenyl phosphite Chemical compound C=1C=CC=CC=1OP([O-])OC1=CC=CC=C1 KUMNEOGIHFCNQW-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- ZUNGGJHBMLMRFJ-UHFFFAOYSA-O ethoxy-hydroxy-oxophosphanium Chemical compound CCO[P+](O)=O ZUNGGJHBMLMRFJ-UHFFFAOYSA-O 0.000 description 1
- ORBFAMHUKZLWSD-UHFFFAOYSA-N ethyl 2-(dimethylamino)benzoate Chemical compound CCOC(=O)C1=CC=CC=C1N(C)C ORBFAMHUKZLWSD-UHFFFAOYSA-N 0.000 description 1
- ZJXZSIYSNXKHEA-UHFFFAOYSA-N ethyl dihydrogen phosphate Chemical compound CCOP(O)(O)=O ZJXZSIYSNXKHEA-UHFFFAOYSA-N 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- NWVVVBRKAWDGAB-UHFFFAOYSA-N hydroquinone methyl ether Natural products COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000007603 infrared drying Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- LRDFRRGEGBBSRN-UHFFFAOYSA-N isobutyronitrile Chemical compound CC(C)C#N LRDFRRGEGBBSRN-UHFFFAOYSA-N 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000002734 metacrylic acid derivatives Chemical class 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- ZQMHJBXHRFJKOT-UHFFFAOYSA-N methyl 2-[(1-methoxy-2-methyl-1-oxopropan-2-yl)diazenyl]-2-methylpropanoate Chemical compound COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC ZQMHJBXHRFJKOT-UHFFFAOYSA-N 0.000 description 1
- CAAULPUQFIIOTL-UHFFFAOYSA-N methyl dihydrogen phosphate Chemical compound COP(O)(O)=O CAAULPUQFIIOTL-UHFFFAOYSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 125000004573 morpholin-4-yl group Chemical group N1(CCOCC1)* 0.000 description 1
- ZFGUAQSDWQIVMM-UHFFFAOYSA-N n'-hydroxy-2-methylbutanimidamide Chemical compound CCC(C)C(N)=NO ZFGUAQSDWQIVMM-UHFFFAOYSA-N 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 125000004957 naphthylene group Chemical group 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- AUONHKJOIZSQGR-UHFFFAOYSA-N oxophosphane Chemical compound P=O AUONHKJOIZSQGR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- LXTZRIBXKVRLOA-UHFFFAOYSA-N padimate a Chemical compound CCCCCOC(=O)C1=CC=C(N(C)C)C=C1 LXTZRIBXKVRLOA-UHFFFAOYSA-N 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- CMPQUABWPXYYSH-UHFFFAOYSA-N phenyl phosphate Chemical compound OP(O)(=O)OC1=CC=CC=C1 CMPQUABWPXYYSH-UHFFFAOYSA-N 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 125000004076 pyridyl group Chemical group 0.000 description 1
- 125000005551 pyridylene group Chemical group 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- RKHXQBLJXBGEKF-UHFFFAOYSA-M tetrabutylphosphanium;bromide Chemical compound [Br-].CCCC[P+](CCCC)(CCCC)CCCC RKHXQBLJXBGEKF-UHFFFAOYSA-M 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 125000005556 thienylene group Chemical group 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 150000007964 xanthones Chemical class 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011787 zinc oxide Substances 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
- G03F7/0045—Photosensitive materials with organic non-macromolecular light-sensitive compounds not otherwise provided for, e.g. dissolution inhibitors
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
-
- 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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Ceramic Engineering (AREA)
- Dispersion Chemistry (AREA)
- Conductive Materials (AREA)
- Materials For Photolithography (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Gas-Filled Discharge Tubes (AREA)
- Parts Printed On Printed Circuit Boards (AREA)
Description
本発明は、基板に導電パターンを形成するために用いられる導電性導電ペーストに関する。 The present invention relates to a conductive conductive paste used for forming a conductive pattern on a substrate.
一般に、回路基板上に電極などの導電パターンを形成する際、有機バインダーに金属粉末を混合した導電性ペーストを、スクリーン印刷法などにより回路基板上に印刷する手法が用いられる（例えば、特許文献１など参照）。 In general, when a conductive pattern such as an electrode is formed on a circuit board, a technique is used in which a conductive paste in which metal powder is mixed with an organic binder is printed on the circuit board by a screen printing method (for example, Patent Document 1). Etc.)
近年、例えばＰＤＰの大画面化、高精細化に伴い、３０インチを超すＰＤＰの回路基板においても、安定して１００μｍ以下の線幅を有する高精細なアドレス電極を形成することが要求されている。しかしながら、このような印刷技術では、大型の回路基板において、高精細な導電パターンを形成することは困難である。 In recent years, for example, with the increase in screen size and definition of PDPs, it has been required to stably form high-definition address electrodes having a line width of 100 μm or less even on PDP circuit boards exceeding 30 inches. . However, with such a printing technique, it is difficult to form a high-definition conductive pattern on a large circuit board.
そこで、感光性導電ペーストを用い、フォトリソグラフィー技術により導電パターンを形成する方法が提案されている（例えば、特許文献２、特許文献３など参照）。このような方法に用いられる感光性導電ペーストにおいて、導電性粉末として銀などの良導電性の貴金属が用いられる。しかしながら、その使用量は大きさに比例するため、特に、大画面のＰＤＰに用いる場合、生産コストが増大するという問題がある。 Therefore, a method of forming a conductive pattern using a photosensitive conductive paste by a photolithography technique has been proposed (see, for example, Patent Document 2 and Patent Document 3). In the photosensitive conductive paste used in such a method, a highly conductive noble metal such as silver is used as the conductive powder. However, since the amount of use is proportional to the size, there is a problem that the production cost increases particularly when used for a large-screen PDP.
このような大面積のＰＤＰに用いる場合などの生産コストの増大を抑えるために、銀粉末の含有量を抑えることが検討される。しかしながら、銀粉末の含有量を抑えると、良好な導電性を得ることが困難であるという問題がある。
本発明は、このような問題を解決するためになされたものであり、銀粉末の含有量を抑え、高精細で、良好な比抵抗値と緻密性を有する導電パターンを形成することが可能な感光性導電ペーストを提供することを目的とする。
In order to suppress an increase in production cost when used in such a large area PDP, it is considered to suppress the content of silver powder. However, if the content of silver powder is suppressed, there is a problem that it is difficult to obtain good conductivity.
The present invention has been made to solve such problems, and can suppress the content of silver powder, and can form a conductive pattern having high definition, good specific resistance value and denseness. An object is to provide a photosensitive conductive paste.
本発明の一態様の感光性導電ペーストは、有機バインダーと、平均粒径が０．１〜２μｍのフレーク状銀粉末と、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、有機溶剤と、ガラスフリットと、を含有することを特徴とするものである。
このような構成により、銀粉末の含有量を抑えながら、高精細で良好な比抵抗値と緻密性を有する導電パターンを形成することが可能となる。
The photosensitive conductive paste of one embodiment of the present invention includes an organic binder, a flaky silver powder having an average particle size of 0.1 to 2 μm, a photopolymerizable monomer, an oxime ester photopolymerization initiator, and an organic solvent. And glass frit.
With such a configuration, it is possible to form a conductive pattern having high definition and good specific resistance value and denseness while suppressing the content of silver powder.
また、本発明の一態様の感光性導電ペーストにおいて、フレーク状銀粉末の含有量は、感光性導電ペーストの２０質量％以上５０質量％未満であることが好ましい。含有量をこの範囲とすることにより、良好な導電性、解像性が得られるとともに、コストダウンが可能となる。 In the photosensitive conductive paste of one embodiment of the present invention, the content of the flaky silver powder is preferably 20% by mass or more and less than 50% by mass of the photosensitive conductive paste. By setting the content within this range, good conductivity and resolution can be obtained, and costs can be reduced.
このような感光性導電ペーストを用いて、導電パターンを形成することができる。そして、このような感光性導電ペーストを用いることにより、高精細で、銀粉末の含有量が少なく、良好な比抵抗値と緻密性を有する導電パターンを形成することができる。 A conductive pattern can be formed using such a photosensitive conductive paste. By using such a photosensitive conductive paste, it is possible to form a conductive pattern having a high definition, a small amount of silver powder, and a good specific resistance value and denseness.
そして、このような導電パターンは、プラズマディスプレイパネルにおいて好適に用いることができる。このようなプラズマディスプレイパネルにより、良好な特性を維持しながらコストダウンを図ることが可能となる。 Such a conductive pattern can be suitably used in a plasma display panel. Such a plasma display panel makes it possible to reduce costs while maintaining good characteristics.
本発明の一態様によれば、銀粉末の含有量を抑え、高精細で、良好な比抵抗値と緻密性を有する導電パターンを形成することが可能となる。 According to one embodiment of the present invention, it is possible to suppress the content of silver powder, and to form a conductive pattern having high definition and good specific resistance and denseness.
本発明の発明者らは、上記課題に対し、鋭意検討した結果、導電体パターン形成に用いるペーストに、導電性粉末としてフレーク状銀粉末および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併用することにより、銀粉末の含有量を抑え、且つ高精細なパターンを形成できることを見出し、本発明を完成するに至った。
具体的には、導電体パターン形成において、フレーク状銀粉末は、他の形状、例えば球状銀粉末と比較して、銀粉末間で接触しやすく、少量でも良好な導電性、即ち良好な比抵抗値、を得ることができる一方、光硬化の際、光の散乱等する効果が大きく塗膜深部までの硬化が難しい。これに対し、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用いることで、少ない露光量で深部硬化を可能にし、高精細な導電体パターンを形成することが可能となる。
As a result of intensive investigations on the above problems, the inventors of the present invention have used a flaky silver powder as a conductive powder and an oxime ester photopolymerization initiator as a photopolymerization initiator in a paste used for forming a conductor pattern. As a result, it was found that the content of silver powder can be suppressed and a high-definition pattern can be formed, and the present invention has been completed.
Specifically, in conductor pattern formation, flaky silver powder is more easily contacted between silver powders than other shapes, for example, spherical silver powder, and has good conductivity even in a small amount, that is, good specific resistance. On the other hand, when photocuring, the effect of scattering light is large, and it is difficult to cure to the deep part of the coating film. On the other hand, by using an oxime ester-based photopolymerization initiator as a photopolymerization initiator, it is possible to cure deep parts with a small exposure amount and to form a high-definition conductor pattern.
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。
本実施形態の感光性導電ペーストは、有機バインダー、フレーク状銀粉末、光重合性モノマー、オキシムエステル系光重合開始剤、有機溶剤およびガラスフリットを含有し、フレーク状銀粉末の含有量は、全体の２０質量％以上５０質量％未満であることを特徴する。
Hereinafter, the photosensitive conductive paste of this embodiment will be described in detail.
The photosensitive conductive paste of this embodiment contains an organic binder, flaky silver powder, a photopolymerizable monomer, an oxime ester photopolymerization initiator, an organic solvent, and a glass frit. The content of the flaky silver powder is It is characterized by being 20 mass% or more and less than 50 mass%.
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、銀粉末を分散し、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 for forming a pattern on a coating film by dispersing silver 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。
なお、（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、以下、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.
In addition, (meth) acrylate is a term which generically refers to acrylate, methacrylate and mixtures thereof, and the same applies to other similar expressions hereinafter.
このようなカルボキシル基含有感光性樹脂およびカルボキシル基含有樹脂は、単独でまたは混合して用いてもよいが、いずれの場合でも、これらは合計で、感光性導電ペースト１００質量部に対して、５〜５０質量部で配合されることが好ましい。これらポリマーの配合量が５質量部未満の場合、形成する塗膜中のこれら樹脂の分布が不均一になりやすく、十分な光硬化性および光硬化深度が得られ難くなり、選択的露光、現像によるパターニングが困難となる。一方、５０質量部を超えた場合、焼成時のパターンのよれや線幅収縮を生じやすくなる。 Such a carboxyl group-containing photosensitive resin and a carboxyl group-containing resin may be used alone or in combination, but in any case, they are 5 in total with respect to 100 parts by mass of the photosensitive conductive paste. It is preferable to be blended at ˜50 parts by mass. When the blending amount of these polymers is less than 5 parts by mass, the distribution of these resins in the coating film to be formed tends to be non-uniform, and it becomes difficult to obtain sufficient photocurability and photocuring depth. Makes patterning difficult. On the other hand, when the amount exceeds 50 parts by mass, the pattern is distorted or the line width is reduced during firing.
また、カルボキシル基含有感光性樹脂およびカルボキシル基含有樹脂としては、それぞれ重量平均分子量が、１，０００〜１００，０００であることが好ましい。これらの樹脂の重量平均分子量が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。 Moreover, as a carboxyl group-containing photosensitive resin and a carboxyl group-containing resin, it is preferable that a weight average molecular weight is 1,000-100,000, respectively. When the weight average molecular weight of these resins is less than 1,000, the adhesion of the coating film during development deteriorates. On the other hand, when it exceeds 100,000, development failure tends to occur. More preferably, it is 5,000-70,000.
そして、これらの樹脂の酸価が、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。 And it is preferable that the acid value of these resin 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 and 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／当量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／当量未満の場合、焼成時に残渣が残りやすくなる。一方、２，０００ｇ／当量を超えた場合、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／当量である。 Further, the double bond equivalent of the carboxyl group-containing photosensitive resin is preferably 350 to 2,000 g / equivalent. When the double bond equivalent of the carboxyl group-containing photosensitive resin is less than 350 g / equivalent, a residue tends to remain during firing. On the other hand, when it exceeds 2,000 g / equivalent, the work margin during development is narrow, and a high exposure amount is required during photocuring. More preferably, it is 400-1500 g / equivalent.
本実施形態の感光性導電ペーストにおけるフレーク状銀粉末は、導電体パターンに導電性を付与するために用いられる。 The flaky silver powder in the photosensitive conductive paste of this embodiment is used for imparting conductivity to the conductor pattern.
ここで、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。 Here, 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).
フレーク状銀粉末の平均粒径は０．１〜２μｍであり、平均厚さＴは０．０１〜１μｍである。平均粒径が０．１μｍ未満である場合、凝集性が高くなり分散が困難となる。一方、２μｍを超えると、焼成後に導電塗膜にピンホールや隙間が生じやすくなり、十分な導電性を得ることが困難となるとともに、導電体パターンエッジの直進性が低下する。より好ましくは０．５〜１μｍである。 The average particle diameter of the flaky silver powder is 0.1 to 2 μm, and the average thickness T is 0.01 to 1 μm. When the average particle diameter is less than 0.1 μm, the cohesiveness becomes high and dispersion becomes difficult. On the other hand, if it exceeds 2 μm, pinholes and gaps are likely to be formed in the conductive coating film after firing, and it becomes difficult to obtain sufficient conductivity, and the straightness of the conductor pattern edge is lowered. More preferably, it is 0.5-1 micrometer.
「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を示す。「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。フレーク状銀粉のアスペクト比としては、３〜５０、より好ましくは５〜３０である。 “Average particle diameter” indicates the average long diameter L of 10 particles measured in the longitudinal direction with a scanning electron microscope. “Average thickness T” indicates the average thickness T of 10 particles measured in the thickness direction with a scanning electron microscope. The aspect ratio of the flaky silver powder is 3 to 50, more preferably 5 to 30.
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個の導電粉末を長手方向に測定した平均を算出することで求められる。
平均厚さＴは、ＳＥＭ（走査型電子顕微鏡）を用いて観察したランダムな１０個の導電粉末を厚さ方向に測定した平均を算出することで求められる。
In addition, an average particle diameter is calculated | required by calculating the average which measured the random 10 conductive powder observed using SEM (scanning electron microscope) in the longitudinal direction.
The average thickness T is obtained by calculating an average obtained by measuring ten random conductive powders observed in a thickness direction using an SEM (scanning electron microscope).
また、フレーク状銀粉末の比表面積は、０．４〜４ｍ２／ｇであることが好ましい。この範囲とすることにより、光の散乱が少なく、塗膜の下部まで十分硬化が進み、現像時の塗膜の剥がれを抑えることができる。より好ましくは０．８〜３ｍ２／ｇである。 The specific surface area of the flaky silver powder is preferably 0.4 to 4 m 2 / g. By setting it as this range, there is little scattering of light, hardening fully progresses to the lower part of a coating film, and it can suppress peeling of the coating film at the time of image development. More preferably, it is 0.8-3 m < 2 > / g.
また、フレーク状銀粉末のタップ密度は、１〜６ｇ／ｃｍ３であることが好ましい。この範囲とすることにより、ペーストの塗布性が良好で緻密な導電体パターンを得ることができる。より好ましくは２〜５ｇ／ｃｍ３である。 Moreover, it is preferable that the tap density of flaky silver powder is 1-6 g / cm < 3 >. By setting it within this range, a dense conductor pattern with good paste applicability can be obtained. More preferably, it is 2-5 g / cm 3 .
このようなフレーク状銀粉末は、感光性導電ペーストの２０質量％以上５０質量％未満となるように配合されることが好ましい。２０質量％未満であると、焼成後の電極がポーラスな状態となり、充分な導電性が得ることが困難となる。また、５０質量％以上であると、コスト高となる。より好ましくは３０質量％以上５０質量％未満である。 Such flaky silver powder is preferably blended so as to be 20% by mass or more and less than 50% by mass of the photosensitive conductive paste. If it is less than 20% by mass, the electrode after firing becomes porous, and it becomes difficult to obtain sufficient conductivity. Further, if it is 50% by mass or more, the cost becomes high. More preferably, it is 30 mass% or more and less than 50 mass%.
本実施形態の感光性導電ペーストにおいて、フレーク状銀粉末とともに、球状銀粉末を用いてもよい。球状銀粉末は、特に制限はしないが平均粒径が０．３〜３μｍ、好ましくは０．５〜２．５μｍの範囲である。なお、本発明において球状銀粉末の形状とは、フレーク状（燐片状）以外の形状を意味し、特に限定はされない。 In the photosensitive conductive paste of this embodiment, spherical silver powder may be used together with the flaky silver powder. The spherical silver powder is not particularly limited, but has an average particle size in the range of 0.3 to 3 μm, preferably 0.5 to 2.5 μm. In the present invention, the shape of the spherical silver powder means a shape other than flakes (flakes) and is not particularly limited.
本実施形態の感光性導電ペーストにおいて、光硬化性の促進および現像性を向上させるために、光重合性モノマーが用いられる。 In the photosensitive conductive paste of this embodiment, a photopolymerizable monomer is used in order to promote photocurability and improve developability.
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, and pentaerythritol triacrylate. , Pentaerythritol tetraacrylate, trimethylolpropane ethylene oxide modified triacrylate, dipentaerythritol pentaacrylate, dipentaerythritol hexaacrylate, and methacrylates corresponding to the above acrylates; phthalic acid, adipic acid, maleic acid, itaconic acid, succinic acid , Polybasic acids such as trimellitic acid and terephthalic acid and hydroxy Mono alkyl (meth) acrylate -, di -, tri -, or the like more polyesters.
なお、光重合性モノマーは、これらに限定されるものではなく、また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。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。 In addition, a photopolymerizable monomer is not limited to these, Moreover, these can be used individually or in combination of 2 or more types. 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は、有機バインダー１００質量部あたり２０〜１００質量部が適当である。光重合性モノマーの配合量が２０質量部未満の場合、十分な光硬化性を得ることが困難となり、一方、１００質量部を超えると、塗膜の深部に比べて表面部の光硬化が速くなるため、硬化ムラを生じやすくなる。 The amount of such a photopolymerizable monomer is appropriately 20 to 100 parts by mass per 100 parts by mass of the organic binder. When the blending amount of the photopolymerizable monomer is less than 20 parts by mass, it is difficult to obtain sufficient photocurability. On the other hand, when it exceeds 100 parts by mass, the photocuring of the surface part is faster than the deep part of the coating film. Therefore, uneven curing is likely to occur.
本実施形態の感光性導電ペーストにおけるオキシムエステル系光重合開始剤は、露光によりラジカルを生成し、光硬化を促進させるために用いられる。特に光重合開始剤として、オキシムエステル系の光重合開始剤を用いることにより、高光感度が得られることから、露光による硬化が困難なフレーク状銀粉を用いた場合であっても、高精細なパターンを形成することができる。 The oxime ester photopolymerization initiator in the photosensitive conductive paste of this embodiment is used for generating radicals by exposure and promoting photocuring. High photosensitivity can be obtained by using an oxime ester-based photopolymerization initiator as a photopolymerization initiator, so even if a flaky silver powder that is difficult to cure by exposure is used, a high-definition pattern can be obtained. Can be formed.
このようなオキシムエステル系光重合開始剤としては、オキシムエステル基を有する光重合開始剤であり、下記一般式で表される化合物、
下記一般式で示される２−（アセチルオキシイミノメチル）チオキサンテン−９−オン、
下記一般式で表される化合物、
下記一般式で表されるカルバゾール構造を有するオキシムエステル化合物や、
特に、好適には、下記一般式で表される化合物を用いることができる。その他、１，２−オクタンジオン,１-[４−フェニルチオ]−,２−（Ｏ−ベンゾイルオキシム）、エタノン，１−[９−エチル−６−（２−メチルベンゾイル）−９Ｈ−カルバゾール−３−イル]−,１−（Ｏ−アセチルオキシム）などを用いることができる。
2- (acetyloxyiminomethyl) thioxanthen-9-one represented by the following general formula:
A compound represented by the following general formula:
An oxime ester compound having a carbazole structure represented by the following general formula,
Particularly preferably, a compound represented by the following general formula can be used. In addition, 1,2-octanedione, 1- [4-phenylthio]-, 2- (O-benzoyloxime), ethanone, 1- [9-ethyl-6- (2-methylbenzoyl) -9H-carbazole-3 -Yl]-, 1- (O-acetyloxime) and the like can be used.
市販品としては、例えば、ＢＡＳＦ社製のＣＧＩ−３２５、イルガキュア（登録商標）ＯＸＥ０１、イルガキュア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, Irgacure (registered trademark) OXE01, Irgacure OXE02, and NCI-831 manufactured by ADEKA.
また、光重合開始剤として、このようなオキシムエステル系開始剤以外の光重合開始剤と併用してもよい。このような光重合開始剤としては、具体例には、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。 Moreover, you may use together with photoinitiators other than such an oxime ester type initiator as a photoinitiator. Specific examples of such a photopolymerization initiator 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-morpholinyl) ) Aminoacetophenones such as phenyl] -1-butanone; 2 Anthraquinones such as methylanthraquinone, 2-ethylanthraquinone, 2-t-butylanthraquinone, 1-chloroanthraquinone; 2,4-dimethylthioxanthone, 2,4-diethylthioxanthone, 2-chlorothioxanthone, 2,4-diisopropylthioxanthone, etc. Thioxanthones; ketones 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-trimethylbenzoyldiph Phosphine oxide such as sulfonyl phosphinate; various peroxides and the like.
市販品としては、例えば、ＢＡＳＦ社製のイルガキュア１８４、イルガキュア８１９、イルガキュア９０７、イルガキュア３６９、イルガキュア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 Lucilin (registered trademark) TPO manufactured by BASF. 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.
これら光重合開始剤の配合割合は、有機バインダー１００質量部あたり０．５〜２０質量部が好ましい。０．５質量部未満であると、十分に光硬化を促進させることが困難となり、２０質量部を超えると、線太りが発生しやすくなり、露光パターンに対する線幅の再現が得られにくくなる。より好ましくは、１〜１５質量部である。 The blending ratio of these photopolymerization initiators is preferably 0.5 to 20 parts by mass per 100 parts by mass of the organic binder. When the amount is less than 0.5 parts by mass, it is difficult to sufficiently promote photocuring. When the amount exceeds 20 parts by mass, line thickening is likely to occur, and it becomes difficult to reproduce the line width with respect to the exposure pattern. More preferably, it is 1-15 mass parts.
このような光重合開始剤は、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。 Such photopolymerization initiators include 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.
また、このような光重合開始剤と併用して、必要に応じて、未硬化の光重合性モノマーを反応させるために、熱重合触媒を用いることができる。この熱重合触媒は、数分から１時間程度の高温におけるエージングにより、未硬化の光重合性モノマーを反応させることができる。 Further, in combination with such a photopolymerization initiator, a thermal polymerization catalyst can be used to react an uncured photopolymerizable monomer as required. This thermal polymerization catalyst can react with an uncured photopolymerizable monomer by aging at a high temperature of about several minutes to 1 hour.
具体的には、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、より好ましいものとしては環境にやさしいノンシアン、ノンハロゲンタイプの１，１’−アゾビス（１−アセトキシ−１−フェニルエタン）が挙げられる。 Specifically, it is a peroxide such as benzoyl peroxide or an azo compound such as isobutyronitrile, preferably 2,2′-azobisisobutyronitrile, 2,2′-azobis-2-methyl. Butyronitrile, 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, and more preferred are rings Friendly non-cyan, halogen-free 1,1'-azobis (1-acetoxy-1-phenylethane) and the like.
本実施態様の感光性導電ペーストにおける有機溶剤は、粘度を調整し、均一な塗膜を形成するために用いられる。 The organic solvent in the photosensitive conductive paste of this embodiment is used for adjusting the viscosity and forming a uniform coating film.
有機溶剤としては、具体的には、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。 Specific examples of the organic solvent include ketones such as methyl ethyl ketone and cyclohexanone; aromatic hydrocarbons such as toluene, xylene, and tetramethylbenzene; cellosolve, methyl cellosolve, carbitol, methylcarbitol, butylcarbitol, and propylene. Glycol ethers such as glycol 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 monoisobutyrate Which esters: 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.
このような有機溶剤（ガラススラリー中の有機溶剤を含む）は、感光性導電ペースト中の有機成分に対して、４０ｗｔ％未満となるように配合されることが好ましい。４０ｗｔ％以上では粘度が低くなり塗布性が悪化する。また、沈降などが発生し、保存安定性が低下する。 Such an organic solvent (including the organic solvent in the glass slurry) is preferably blended so as to be less than 40 wt% with respect to the organic component in the photosensitive conductive paste. If it is 40 wt% or more, the viscosity will be low and the coating property will be deteriorated. In addition, sedimentation occurs and storage stability is reduced.
ここで、有機成分とは、感光性導電ペースト中に配合される有機化合物（有機金属化合物を含む）のことである。具体的には、有機バインダー、光重合性モノマー、光重合開始剤、有機溶剤の他、分散剤、安定剤などすべての有機化合物である。 Here, the organic component is an organic compound (including an organometallic compound) blended in the photosensitive conductive paste. Specifically, it is all organic compounds such as an organic binder, a photopolymerizable monomer, a photopolymerization initiator, an organic solvent, a dispersant, and a stabilizer.
本実施態様の感光性導電ペーストにおけるガラスフリットは、焼成後の導電体パターンの基板への密着性を向上させるために用いられる。 The glass frit in the photosensitive conductive paste of this embodiment is used for improving the adhesion of the baked conductor pattern to the substrate.
ガラスフリットの平均粒径（Ｄ５０）は、０．３〜１．５μｍとする。平均粒径（Ｄ５０）が０．３μｍ未満であると、収率が著しく低下しコスト高となり、１．５μｍを超えると、薄膜の形成や、焼成時の均一な収縮が困難となり、ライン形状や緻密性が劣化する。 The average particle size (D50) of the glass frit is 0.3 to 1.5 μm. When the average particle size (D50) is less than 0.3 μm, the yield is remarkably reduced and the cost is increased. When the average particle size is more than 1.5 μm, it is difficult to form a thin film or uniformly shrink during firing. Density deteriorates.
また、ガラスフリットの軟化点は、４８０〜６２０℃とする。ガラス軟化点が４８０℃未満であると、得られる導電体パターンにおいて十分な緻密性を得ることが困難となり、６２０℃を超えると抵抗値が上昇する。 The softening point of the glass frit is 480 to 620 ° C. When the glass softening point is less than 480 ° C., it is difficult to obtain sufficient denseness in the obtained conductor pattern, and when it exceeds 620 ° C., the resistance value increases.
このようなガラスフリットとしては、酸化鉛、酸化ビスマス、酸化亜鉛、酸化リチウム、またはアルカリホウケイ酸塩を主成分とするものが好適に用いられる。 As such a glass frit, a material mainly composed of lead oxide, bismuth oxide, zinc oxide, lithium oxide, or alkali borosilicate is preferably used.
このようなガラスフリットの配合量は、銀粉末１００質量部に対して、０．０１〜３５質量部であることが好ましい。０．０１質量部未満であると、焼成後の導電体パターンの基板への良好な密着性を得ることが困難となる。一方、３５質量部を超えると、良好な緻密性と比抵抗値を得ることが困難となる。より好ましくは１〜２０質量部である。さらに、このようなガラスフリットの熱膨張係数α３００は、６０〜１１０×１０−７であることが好ましい。 It is preferable that the compounding quantity of such a glass frit is 0.01-35 mass parts with respect to 100 mass parts of silver powder. If it is less than 0.01 part by mass, it becomes difficult to obtain good adhesion to the substrate of the conductive pattern after firing. On the other hand, when it exceeds 35 parts by mass, it becomes difficult to obtain good density and specific resistance. More preferably, it is 1-20 mass parts. Furthermore, the thermal expansion coefficient α300 of such a glass frit is preferably 60 to 110 × 10 −7 .
このような感光性導電ペーストにおいて、さらに、感光性導電ペースト中のガラスフリットを均一に分散するために、分散剤を添加することができる。 In such a photosensitive conductive paste, a dispersant can be further added to uniformly disperse the glass frit in the photosensitive conductive paste.
分散剤としては、ガラスフリットを均一に分散できるものであればよく、特に限定されるものではない。例えば、ポリカルボン酸型高分子界面活性剤、変性アクリル系ブロック共重合体、顔料親和性基を有するアクリル共重合物、塩基性或いは酸性の顔料吸着基を有するブロック共重合物、顔料親和性基を有する変性ポリアルコキシレート、ポリアミノアマイド塩とポリエステル、極性酸エステルと高分子アルコールの組み合わせ、酸性ポリマーのアルキルアンモニウム塩、顔料親和性基を有する高分子量ブロック共重合体、特殊変性ウレアなどが挙げられるが、特にこれらに限定されるものではない。また、これらの分散剤を単独でまたは２種以上を組み合わせて用いることができる。 The dispersant is not particularly limited as long as it can uniformly disperse the glass frit. For example, polycarboxylic acid type polymer surfactant, modified acrylic block copolymer, acrylic copolymer having pigment affinity group, block copolymer having basic or acidic pigment adsorbing group, pigment affinity group Modified polyalkoxylates having polyamines, polyaminoamide salts and polyesters, combinations of polar acid esters and high molecular alcohols, alkylammonium salts of acidic polymers, high molecular weight block copolymers having pigment affinity groups, special modified ureas, and the like However, it is not particularly limited to these. Moreover, these dispersing agents can be used individually or in combination of 2 or more types.
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銀粉末やガラスフリットなどの無機粉末の成分である金属あるいは酸化物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, there can be used a compound having an effect of complexing with a metal or oxide which is a component of inorganic powder such as silver powder or glass frit in the photosensitive conductive paste, or salt formation.
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。 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) ) Acids such as various phosphate compounds (inorganic phosphoric acid, organic phosphoric acid) such as acid phosphate and di (2-methacryloyloxyethyl) acid phosphate.
なお、安定剤はこれらに限定されるものではなく、また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。このような安定剤は、無機粉末１００質量部に対して０．１〜１０質量部の割合で添加することが好ましい。 In addition, a stabilizer is not limited to these, Moreover, these can be used individually or in combination of 2 or more types. Such a stabilizer is preferably added at a ratio of 0.1 to 10 parts by mass with respect to 100 parts by mass of the inorganic powder.
さらに本実施形態の感光性導電ペーストにおいて、必要に応じて、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。さらに、必要に応じて、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, in the photosensitive conductive paste of the present embodiment, if necessary, 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 are blended. can do. Furthermore, a known antioxidant or a thermal polymerization inhibitor for improving the thermal stability during storage may be added as necessary.
本実施形態において、こ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る。このとき、攪拌機により攪拌後、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。なお、ガラスフリットを微粒子化し均一に分散させるために、予めガラススラリーを調製して混合することが好ましい。 In this embodiment, the photosensitive electrically conductive paste comprised in this way is prepared by mixing each component. At this time, after stirring with a stirrer, it can be paste-formed by kneading with a three-roll mill or the like. In order to make the glass frit fine and uniformly disperse, it is preferable to prepare and mix the glass slurry in advance.
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、例えばＰＤＰの前面基板となるガラス基板などの基板に塗布し、塗膜を形成する。 The photosensitive conductive paste prepared in this way is applied to a substrate such as a glass substrate serving as a front substrate of a PDP 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、有機溶剤を蒸発させ、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塗布、乾燥して、ドライフィルムを形成した場合には、ドライフィルムを基板上にラミネートしてもよい。 Next, in order to obtain a touch-drying property, the obtained coating film is dried, for example, at about 70 to 120 ° C. for about 5 to 40 minutes in a hot air circulation drying oven, a far infrared drying oven, etc., and the organic solvent is evaporated. A tack-free coating (dry coating) is formed. At this time, when a photosensitive conductive paste is previously applied on a film and dried to form a dry film, the dry film may be laminated on the substrate.
そして、得られた乾燥塗膜をパターン露光する。露光方法としては、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、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１００〜８００ｍＪ／ｃｍ２程度が好ましい。 The resulting dried coating film is subjected to pattern exposure. As an exposure method, contact exposure and non-contact exposure using a negative mask having a predetermined exposure pattern are possible. As the exposure light source, 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 amount is preferably about 100 to 800 mJ / cm 2 .
さらに、所定パターンに露光された塗膜を現像する。現像方法としてはスプレー法、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の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い。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、珪酸ナトリウムなど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などのアミン水溶液、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。 Furthermore, the coating film exposed to a predetermined pattern is developed. As a developing method, a spray method, a dipping method or the like is used. As the developer, it is only necessary that the carboxyl group of the carboxyl group-containing resin of the photosensitive conductive paste is saponified and the uncured portion (unexposed portion) can be removed. For example, an aqueous alkali metal solution such as sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, or sodium silicate, an aqueous amine solution such as monoethanolamine, diethanolamine, or triethanolamine, particularly a dilute solution having a concentration of about 1.5 wt% or less. An alkaline aqueous solution is preferably used. Moreover, it is preferable to perform washing with water and acid neutralization in order to remove an unnecessary developer after development.
そして、パターンが現像された基板を焼成し、導電パターンを形成する。焼成条件は、例えば、空気雰囲気下または窒素雰囲気下で、約４００〜６００℃とすることができる。このとき、昇温速度は、２０℃／分以下に設定することが好ましい。 And the board | substrate with which the pattern was developed is baked and a conductive pattern is formed. Firing conditions can be, for example, about 400 to 600 ° C. in an air atmosphere or a nitrogen atmosphere. At this time, it is preferable to set the heating rate to 20 ° C./min or less.
このようにして、高精細で、銀粉末の含有量が少なく、良好な比抵抗値と緻密性を有する導電パターンを形成することができる。そして、得られた導電パターンは、プラズマディスプレイなどに好適に用いられ、良好な特性を維持しながらコストダウンを図ることが可能となる。 In this way, it is possible to form a conductive pattern having high definition, low silver powder content, and good specific resistance and denseness. The obtained conductive pattern is suitably used for a plasma display or the like, and it is possible to reduce the cost while maintaining good characteristics.
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。 Hereinafter, although an Example and a comparative example are shown and this embodiment is demonstrated concretely, this invention is not limited to these Examples.
（有機バインダーの合成）
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とメタクリル酸を０．７６：０．２４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ニトリルを入れ、窒素雰囲気下、８０℃で２〜６時間攪拌し、樹脂溶液を得た。
(Synthesis of organic binder)
A flask equipped with a thermometer, a stirrer, a dropping funnel, and a reflux condenser is charged with methyl methacrylate and methacrylic acid in a molar ratio of 0.76: 0.24, dipropylene glycol monomethyl ether as a solvent, and azobisiso as a catalyst. Butyronitrile was added and stirred at 80 ° C. for 2 to 6 hours under a nitrogen atmosphere to obtain a resin solution.
この樹脂溶液を冷却し、重合禁止剤としてメチルハイドロキノン、触媒としてテトラブチルホスホニウムブロマイドを用い、グリシジルメタクリレートを、９５〜１０５℃で１６時間の条件で、上記樹脂のカルボキシル基１モルに対し０．１２モルの割合の付加モル比で付加反応させ、冷却後取り出し、有機バインダーを得た。 The resin solution was cooled, methylhydroquinone as a polymerization inhibitor, tetrabutylphosphonium bromide as a catalyst, and glycidyl methacrylate at a temperature of 95 to 105 ° C. for 16 hours to 0.12 mol per mol of the carboxyl group of the resin. Addition reaction was carried out at an addition molar ratio of a molar ratio, and the mixture was taken out after cooling to obtain an organic binder.
得られた有機バインダーは、重量平均分子量が約１０，０００、固形分酸価が５９ｍｇＫＯＨ／ｇ、二重結合当量が９５０であった。なお、重量平均分子量の測定は、ポンプＬＣ−６ＡＤ（島津製作所社製）とカラムＳｈｏｄｅｘ（登録商標）ＫＦ−８０４、ＫＦ−８０３、ＫＦ−８０２（昭和電工社製）を三本つないだ高速液体クロマトグラフィーにより測定した。 The obtained organic binder had a weight average molecular weight of about 10,000, a solid content acid value of 59 mgKOH / g, and a double bond equivalent of 950. The weight average molecular weight is measured by a pump LC-6AD (manufactured by Shimadzu Corp.) and a column Shodex (registered trademark) KF-804, KF-803, KF-802 (manufactured by Showa Denko KK). Measured by chromatography.
（ガラススラリーの調製）
ガラスフリットと、有機溶剤と、分散剤を混合し、これをビーズミルにより湿式分散することにより、ガラスフリット６５ｗｔ％のガラススラリーを調製した。
(Preparation of glass slurry)
Glass frit, an organic solvent, and a dispersing agent were mixed and wet-dispersed with a bead mill to prepare a glass slurry having a glass frit of 65 wt%.
（感光性導電ペーストの調製）
得られた有機バインダー及びガラススラリーを用いて、各成分を表１に示す組成比にて配合し、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及び比較例１〜５の各感光性導電ペーストを調製した。
(Preparation of photosensitive conductive paste)
Using the obtained organic binder and glass slurry, each component was blended at the composition ratio shown in Table 1, and after stirring with a stirrer, it was kneaded with a three-roll mill to form a paste. Each photosensitive electrically conductive paste of Comparative Examples 1-5 was prepared.
＊１：燐酸エステル
＊２：Ｍ−３５０（東亞合成化学社製）
＊３−１：平均粒径＝０．７６、平均厚さＴ＝０．５２μｍ、アスペクト比＝１．５
＊３−２：平均粒径＝２．４６、平均厚さＴ＝１．９２μｍ、アスペクト比＝１．３
＊４：平均粒径＝０．６６、平均厚さＴ＝０．１０μｍ、アスペクト比＝６．６
＊５：平均粒径＝２．３３、平均厚さＴ＝０．１７μｍ、アスペクト比＝１３．７
＊６：イルガキュア３６９（ＢＡＳＦ社製）
＊７：オキシムエステル系光重合開始剤 ＮＣＩ−８３１（ＡＤＥＫＡ社製）
＊８：エロジル＃３８０（日本アエロジル社製）
＊９：モダフロー（登録商標 モンサントケミカル社製）
＊１０：石油系溶剤
* 1: Phosphate ester * 2: M-350 (Toagosei Co., Ltd.)
* 3-1: Average particle size = 0.76, average thickness T = 0.52 μm, aspect ratio = 1.5
* 3-2: Average particle diameter = 2.46, average thickness T = 1.92 μm, aspect ratio = 1.3
* 4: Average particle size = 0.66, average thickness T = 0.10 μm, aspect ratio = 6.6
* 5: Average particle size = 2.33, average thickness T = 0.17 μm, aspect ratio = 13.7
* 6: Irgacure 369 (BASF)
* 7: Oxime ester photopolymerization initiator NCI-831 (manufactured by ADEKA)
* 8: Erosil # 380 (Nippon Aerosil Co., Ltd.)
* 9: Modaflow (registered trademark, manufactured by Monsanto Chemical Co., Ltd.)
* 10: Petroleum solvent
（５０ｉｎｃｈライン抵抗値評価）
先ず、このようにして調製された各感光性導電ペーストを用いて、評価用導電パターンを作成した。
(50 inch line resistance value evaluation)
First, the conductive pattern for evaluation was created using each photosensitive electrically conductive paste prepared in this way.
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、ウエット膜厚が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。 Each photosensitive conductive paste was applied on the entire surface of a 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.
次に、光源としてショートアークランプを用い、ネガマスクを介して、表２に示す条件で、フォトマスク設計７０／８０／９０／１００／１１０／１２０μｍでパターン露光した後、０．４ｗｔ％の炭酸ナトリウム水溶液を用いて現像を行い、水洗した。 Next, after using a short arc lamp as a light source and pattern exposure with a photomask design 70/80/90/100/110/120 μm through a negative mask under the conditions shown in Table 2, 0.4 wt% sodium carbonate Development was performed using an aqueous solution and washed with water.
このようにして線長６２３ｍｍ（５０ｉｎｃｈライン長）のパターンが形成された基板を、空気雰囲気下にて５９０℃で１０分間、昇温速度１４℃／ｍｉｎで焼成し、評価用導電パターンを作成した。 Thus, the board | substrate with which the pattern of line length 623mm (50 inch line length) was formed was baked at 590 degreeC for 10 minutes and the temperature increase rate of 14 degreeC / min in air atmosphere, and the conductive pattern for evaluation was created. .
得られた各評価用導電パターンにおいて、焼成後線幅を測定し、併せてミリオームテスター（ＨＩＯＫＩ３５４０ｍΩ、ＨＩＯＫＩ社製）により、ライン抵抗値を測定した。焼成後線幅に対するライン抵抗値をプロットし、近似曲線より、焼成線幅８０／９０／１００μｍにおけるライン抵抗値を求めた。測定結果を表２に示す。 In each of the obtained conductive patterns for evaluation, the line width after firing was measured, and the line resistance value was also measured with a milliohm tester (HIOKI 3540 mΩ, manufactured by HIOKI). The line resistance value against the line width after firing was plotted, and the line resistance value at the firing line width of 80/90/100 μm was determined from the approximate curve. The measurement results are shown in Table 2.
（比抵抗値評価）
このようにして調製された各感光性導電ペーストを用いて、同様にして０．４×１０ｃｍのラインパターンを作成した。
(Specific resistance evaluation)
Using each photosensitive conductive paste thus prepared, a 0.4 × 10 cm line pattern was created in the same manner.
各ラインパターンの膜厚を、表面粗さ計（ＳＥ７００、小坂研究所製）を用いて測定するとともに、ラインパターンにおける抵抗値をミリオームハイテスター（ＨＩＯＫＩ３５４０ｍΩ、ＨＩＯＫＩ社製）により測定し、比抵抗値を算出した。
これらの測定結果を表２に示す。
The film thickness of each line pattern is measured using a surface roughness meter (SE700, manufactured by Kosaka Laboratories), and the resistance value in the line pattern is measured with a milliohm high tester (HIOKI3540 mΩ, manufactured by HIOKI). Was calculated.
These measurement results are shown in Table 2.
（パターン形成性評価）
このようにして調製された各感光性導電ペーストを用いて、各線幅のライン／スペースのパターンを同様に現像し、現像後の膜厚を表面粗さ計で測定した。これを焼成して、得られた焼成パターンの膜厚を同様に測定し、各線幅のライン／スペースのライン残存性とスペースの抜け性を評価した。
共に問題のないライン／スペースの線幅（μｍ）をパターン形成性の評価結果とした。
また、パターン直進性についても評価した。
(Pattern formability evaluation)
Using each photosensitive conductive paste thus prepared, line / space patterns with respective line widths were similarly developed, and the film thickness after development was measured with a surface roughness meter. This was fired, and the film thickness of the obtained fired pattern was measured in the same manner, and the line survivability of the line / space of each line width and the detachability of the space were evaluated.
The line width (μm) of the line / space that has no problem in both cases was used as the evaluation result of the pattern formability.
In addition, pattern straightness was also evaluated.
このように、本実施形態の感光性導電ペーストを用いた実施例１、２は、５０ｉｎｃｈライン抵抗値評価、比抵抗値評価、及びパターン形成性評価とも良好な結果が得られていることがわかる。
まず、粒径の小さい球状銀粉末を用いた比較例１は実施例１に比較し、５０ｉｎｃｈライン抵抗値及び比抵抗値が高く、また、粒径の大きい球状銀粉末を用いた比較例２は更に５０ｉｎｃｈライン抵抗値及び比抵抗値が高かった。また、球状、フレーク状何れも粒径の大きい銀粉末を用いた場合（比較例２、比較例３）、パターン直進性においてギザツキが確認され、解像性も悪かった。
これに対し、一定の粒径のフレーク状銀粉末を用いた実施例１は、比較例１、比較例２及び比較例３と同じ銀含有率で低いライン抵抗値が得られている。また、実施例２のとおり、銀含有率を低減しても同等のライン抵抗値を得ることができる。また、実施例１、２はパターン直進性や解像性も良好であり、パターン形成性を向上させることが可能となる。
As described above, in Examples 1 and 2 using the photosensitive conductive paste of the present embodiment, it is understood that good results are obtained in 50 inch line resistance value evaluation, specific resistance value evaluation, and pattern formability evaluation. .
First, Comparative Example 1 using a spherical silver powder having a small particle size has a higher 50-inch line resistance value and specific resistance value than Example 1, and Comparative Example 2 using a spherical silver powder having a large particle size is Furthermore, the 50-inch line resistance value and the specific resistance value were high. Further, when silver powder having a large particle size was used for both spherical and flaky shapes (Comparative Example 2 and Comparative Example 3), the pattern straightness was confirmed and the resolution was poor.
On the other hand, in Example 1 using the flaky silver powder having a constant particle size, a low line resistance value was obtained with the same silver content as Comparative Example 1, Comparative Example 2 and Comparative Example 3. Further, as in Example 2, even if the silver content is reduced, an equivalent line resistance value can be obtained. In addition, Examples 1 and 2 have good pattern rectilinearity and resolution, and can improve pattern formation.
また、オキシムエステル系光重合開始剤を用いていない比較例４、５は、現像による減膜が顕著に認められ、比較例４はパターンが残存せず、比較例５はパターン直進性が悪くライン抵抗値も高かった。
これに対し、オキシムエステル系光重合開始剤を用いている実施例１、２は、同じ銀含有率であっても、パターン直進性が良好であり、ライン抵抗値も低くなる。
Further, in Comparative Examples 4 and 5 in which no oxime ester photopolymerization initiator was used, film thickness reduction due to development was remarkably observed, Comparative Example 4 had no pattern remaining, and Comparative Example 5 had poor linearity in the pattern. The resistance value was also high.
In contrast, in Examples 1 and 2 using the oxime ester photopolymerization initiator, the pattern straightness is good and the line resistance value is low even if the silver content is the same.
Claims (3)
前記有機バインダーは、酸価が５０〜２５０ｍｇＫＯＨ／ｇであるカルボキシル基含有樹脂であり、
前記フレーク状銀粉末の含有量は、全体の２０質量％以上５０質量％未満であることを特徴とする感光性導電ペースト。 And organic binder, containing an average particle diameter of 0.1~2μm flaky silver powder, a photopolymerizable monomer, and oxime ester-based photopolymerization initiator, an organic solvent, glass frit, and
The organic binder is a carboxyl group-containing resin having an acid value of 50 to 250 mgKOH / g,
Content of the said flaky silver powder is 20 to less than 50 mass% of the whole, The photosensitive electrically conductive paste characterized by the above-mentioned.
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