JPWO2014171387A1 - Conductive pressure-sensitive adhesive sheet, method for producing the same, and electronic terminal obtained using the same - Google Patents
Conductive pressure-sensitive adhesive sheet, method for producing the same, and electronic terminal obtained using the same Download PDFInfo
- Publication number
- JPWO2014171387A1 JPWO2014171387A1 JP2014544280A JP2014544280A JPWO2014171387A1 JP WO2014171387 A1 JPWO2014171387 A1 JP WO2014171387A1 JP 2014544280 A JP2014544280 A JP 2014544280A JP 2014544280 A JP2014544280 A JP 2014544280A JP WO2014171387 A1 JPWO2014171387 A1 JP WO2014171387A1
- Authority
- JP
- Japan
- Prior art keywords
- conductive
- sensitive adhesive
- adhesive sheet
- pressure
- mass
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 126
- 238000004519 manufacturing process Methods 0.000 title claims description 32
- 239000000853 adhesive Substances 0.000 claims abstract description 103
- 230000001070 adhesive effect Effects 0.000 claims abstract description 103
- 229920000728 polyester Polymers 0.000 claims abstract description 67
- 239000002245 particle Substances 0.000 claims abstract description 66
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 57
- 239000000463 material Substances 0.000 claims abstract description 54
- 238000007747 plating Methods 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 49
- 239000010410 layer Substances 0.000 claims abstract description 43
- 238000007772 electroless plating Methods 0.000 claims abstract description 38
- 239000000758 substrate Substances 0.000 claims description 76
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 63
- 239000012790 adhesive layer Substances 0.000 claims description 37
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 30
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 28
- 229910052759 nickel Inorganic materials 0.000 claims description 28
- 239000010949 copper Substances 0.000 claims description 27
- 229910052802 copper Inorganic materials 0.000 claims description 26
- 239000000178 monomer Substances 0.000 claims description 24
- 229920000058 polyacrylate Polymers 0.000 claims description 14
- 238000009713 electroplating Methods 0.000 claims description 8
- 238000010030 laminating Methods 0.000 claims description 4
- 230000000379 polymerizing effect Effects 0.000 claims description 4
- 239000004020 conductor Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 53
- 239000002585 base Substances 0.000 description 36
- 239000000243 solution Substances 0.000 description 35
- 238000002360 preparation method Methods 0.000 description 34
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 26
- -1 organic acid salts Chemical class 0.000 description 25
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 20
- 239000011347 resin Substances 0.000 description 17
- 229920005989 resin Polymers 0.000 description 17
- 229910052751 metal Inorganic materials 0.000 description 16
- 239000002184 metal Substances 0.000 description 16
- 239000007787 solid Substances 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 239000000835 fiber Substances 0.000 description 15
- 239000000123 paper Substances 0.000 description 13
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 12
- 229920002554 vinyl polymer Polymers 0.000 description 12
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 11
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 11
- 239000003431 cross linking reagent Substances 0.000 description 11
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 11
- 238000005406 washing Methods 0.000 description 11
- 229920006243 acrylic copolymer Polymers 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 10
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 239000011888 foil Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 229910000365 copper sulfate Inorganic materials 0.000 description 7
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 6
- 229910001369 Brass Inorganic materials 0.000 description 6
- 239000010951 brass Substances 0.000 description 6
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 6
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 6
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 6
- 239000003381 stabilizer Substances 0.000 description 6
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 5
- 125000000217 alkyl group Chemical group 0.000 description 5
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 239000001509 sodium citrate Substances 0.000 description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 5
- 235000011083 sodium citrates Nutrition 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 239000001119 stannous chloride Substances 0.000 description 5
- 235000011150 stannous chloride Nutrition 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 4
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 4
- 239000003522 acrylic cement Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 235000011187 glycerol Nutrition 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000003505 polymerization initiator Substances 0.000 description 4
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 4
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 235000019270 ammonium chloride Nutrition 0.000 description 3
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 3
- 239000012964 benzotriazole Substances 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000008139 complexing agent Substances 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 239000011889 copper foil Substances 0.000 description 3
- PYRZPBDTPRQYKG-UHFFFAOYSA-N cyclopentene-1-carboxylic acid Chemical compound OC(=O)C1=CCCC1 PYRZPBDTPRQYKG-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000012948 isocyanate Substances 0.000 description 3
- 150000002513 isocyanates Chemical class 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- GHPYJLCQYMAXGG-WCCKRBBISA-N (2R)-2-amino-3-(2-boronoethylsulfanyl)propanoic acid hydrochloride Chemical compound Cl.N[C@@H](CSCCB(O)O)C(O)=O GHPYJLCQYMAXGG-WCCKRBBISA-N 0.000 description 2
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 2
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- DLDJFQGPPSQZKI-UHFFFAOYSA-N but-2-yne-1,4-diol Chemical compound OCC#CCO DLDJFQGPPSQZKI-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000003002 pH adjusting agent Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 2
- 229940081974 saccharin Drugs 0.000 description 2
- 235000019204 saccharin Nutrition 0.000 description 2
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 2
- 150000003852 triazoles Chemical class 0.000 description 2
- DIIIISSCIXVANO-UHFFFAOYSA-N 1,2-Dimethylhydrazine Chemical compound CNNC DIIIISSCIXVANO-UHFFFAOYSA-N 0.000 description 1
- JWYVGKFDLWWQJX-UHFFFAOYSA-N 1-ethenylazepan-2-one Chemical compound C=CN1CCCCCC1=O JWYVGKFDLWWQJX-UHFFFAOYSA-N 0.000 description 1
- XLPJNCYCZORXHG-UHFFFAOYSA-N 1-morpholin-4-ylprop-2-en-1-one Chemical compound C=CC(=O)N1CCOCC1 XLPJNCYCZORXHG-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
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 description 1
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 1
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 1
- MZZYGYNZAOVRTG-UHFFFAOYSA-N 2-hydroxy-n-(1h-1,2,4-triazol-5-yl)benzamide Chemical compound OC1=CC=CC=C1C(=O)NC1=NC=NN1 MZZYGYNZAOVRTG-UHFFFAOYSA-N 0.000 description 1
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
- 125000004200 2-methoxyethyl group Chemical group [H]C([H])([H])OC([H])([H])C([H])([H])* 0.000 description 1
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 description 1
- SXIFAEWFOJETOA-UHFFFAOYSA-N 4-hydroxy-butyl Chemical group [CH2]CCCO SXIFAEWFOJETOA-UHFFFAOYSA-N 0.000 description 1
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 229920006310 Asahi-Kasei Polymers 0.000 description 1
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 1
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- OFLXLNCGODUUOT-UHFFFAOYSA-N acetohydrazide Chemical compound C\C(O)=N\N OFLXLNCGODUUOT-UHFFFAOYSA-N 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- BIVUUOPIAYRCAP-UHFFFAOYSA-N aminoazanium;chloride Chemical compound Cl.NN BIVUUOPIAYRCAP-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- VDTVZBCTOQDZSH-UHFFFAOYSA-N borane N-ethylethanamine Chemical compound B.CCNCC VDTVZBCTOQDZSH-UHFFFAOYSA-N 0.000 description 1
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
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- 238000012662 bulk polymerization Methods 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- DOBRDRYODQBAMW-UHFFFAOYSA-N copper(i) cyanide Chemical compound [Cu+].N#[C-] DOBRDRYODQBAMW-UHFFFAOYSA-N 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 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
- 238000013461 design Methods 0.000 description 1
- PEVJCYPAFCUXEZ-UHFFFAOYSA-J dicopper;phosphonato phosphate Chemical compound [Cu+2].[Cu+2].[O-]P([O-])(=O)OP([O-])([O-])=O PEVJCYPAFCUXEZ-UHFFFAOYSA-J 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- MCPKSFINULVDNX-UHFFFAOYSA-N drometrizole Chemical compound CC1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 MCPKSFINULVDNX-UHFFFAOYSA-N 0.000 description 1
- BXKDSDJJOVIHMX-UHFFFAOYSA-N edrophonium chloride Chemical compound [Cl-].CC[N+](C)(C)C1=CC=CC(O)=C1 BXKDSDJJOVIHMX-UHFFFAOYSA-N 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000010556 emulsion polymerization method Methods 0.000 description 1
- IFQUWYZCAGRUJN-UHFFFAOYSA-N ethylenediaminediacetic acid Chemical compound OC(=O)CNCCNCC(O)=O IFQUWYZCAGRUJN-UHFFFAOYSA-N 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011086 glassine Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000012493 hydrazine sulfate Substances 0.000 description 1
- 229910000377 hydrazine sulfate Inorganic materials 0.000 description 1
- 150000002429 hydrazines Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 239000002655 kraft paper Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000006078 metal deactivator Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 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
- HDZGCSFEDULWCS-UHFFFAOYSA-N monomethylhydrazine Chemical compound CNN HDZGCSFEDULWCS-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
- 229940088644 n,n-dimethylacrylamide Drugs 0.000 description 1
- YLGYACDQVQQZSW-UHFFFAOYSA-N n,n-dimethylprop-2-enamide Chemical compound CN(C)C(=O)C=C YLGYACDQVQQZSW-UHFFFAOYSA-N 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 235000001968 nicotinic acid Nutrition 0.000 description 1
- 229960003512 nicotinic acid Drugs 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- HKOOXMFOFWEVGF-UHFFFAOYSA-N phenylhydrazine Chemical compound NNC1=CC=CC=C1 HKOOXMFOFWEVGF-UHFFFAOYSA-N 0.000 description 1
- 229940067157 phenylhydrazine Drugs 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229960003975 potassium Drugs 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 239000001508 potassium citrate Substances 0.000 description 1
- 229960002635 potassium citrate Drugs 0.000 description 1
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 1
- 235000011082 potassium citrates Nutrition 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 102220269348 rs61747367 Human genes 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 238000010558 suspension polymerization method Methods 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000009823 thermal lamination Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 238000009692 water atomization Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/21—Paper; Textile fabrics
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- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K2003/0862—Nickel
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/314—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive layer and/or the carrier being conductive
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
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- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/20—Presence of organic materials
- C09J2400/26—Presence of textile or fabric
- C09J2400/263—Presence of textile or fabric in the substrate
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- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
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- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Laminated Bodies (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Adhesive Tapes (AREA)
- Health & Medical Sciences (AREA)
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Abstract
本発明の導電性粘着シートは、導電性基材の少なくとも片面に、導電性粘着剤層を有する導電性粘着シートであって、前記導電性基材が、湿式であるポリエステル系不織布基材に、無電解メッキ処理を含むメッキ処理を施すことによって得られた導電性基材であり、前記導電性粘着剤層が、前記導電性粘着剤層の全体に対して、導電性粒子を３質量％〜５０質量％の範囲で含有するものであることを特徴とする導電性粘着シートに関するものである。The conductive pressure-sensitive adhesive sheet of the present invention is a conductive pressure-sensitive adhesive sheet having a conductive pressure-sensitive adhesive layer on at least one surface of a conductive base material, and the conductive base material is a wet polyester-based nonwoven fabric base material. It is a conductive base material obtained by performing a plating process including an electroless plating process, and the conductive pressure-sensitive adhesive layer has a conductive particle content of 3% by mass to the whole of the conductive pressure-sensitive adhesive layer. It is related with the electroconductive adhesive sheet characterized by containing in the range of 50 mass%.
Description
本発明は、例えば携帯電子端末等の電子機器等の製造に使用可能な導電性粘着シートに関する。 The present invention relates to a conductive pressure-sensitive adhesive sheet that can be used for manufacturing electronic devices such as portable electronic terminals.
近年、通信機器等の電子機器の小型化、薄型化及び高性能化に伴って高集積化が進んでいる。前記電子機器の製造の際には、電子機器から発生されうる電磁波を遮へいしたり、任意の部位に帯電防止性を付与すること等を目的として、導電性粘着シートを使用する場合が多い。 In recent years, electronic devices such as communication devices have been highly integrated with miniaturization, thinning, and high performance. In the manufacture of the electronic device, a conductive adhesive sheet is often used for the purpose of shielding electromagnetic waves that can be generated from the electronic device or imparting antistatic properties to an arbitrary site.
前記導電性粘着シートとしては、例えば金属箔からなる導電性基材上に、導電性フィラーを含有する導電性粘着剤層を有する粘着シートが知られている（例えば、特許文献１及び２参照。）。
As the conductive pressure-sensitive adhesive sheet, a pressure-sensitive adhesive sheet having a conductive pressure-sensitive adhesive layer containing a conductive filler on a conductive base material made of, for example, metal foil is known (see, for example,
前記したような金属箔を用いた導電性粘着シートは、どうしても柔軟性の点で十分でないため、被着体の表面に微小な段差がある場合に、前記段差部に追従することができず、被着体と粘着剤層との界面に空隙を形成してしまう場合があった。 Since the conductive adhesive sheet using the metal foil as described above is not sufficient in terms of flexibility, when there is a minute step on the surface of the adherend, the step portion cannot be followed, In some cases, voids were formed at the interface between the adherend and the pressure-sensitive adhesive layer.
一方、産業界からは、前記導電性粘着シートを、被着体の誤った位置に貼付してしまった場合に、その貼付直後であれば容易に剥離できるレベルのリワーク性が求められている。 On the other hand, there is a demand from the industry for a level of reworkability that can be easily peeled off immediately after application when the conductive adhesive sheet is attached to an incorrect position of an adherend.
しかし、前記したような導電性粘着シートは、前記リワーク性の点で十分でない場合が多く、再利用し貼り直しすることができない場合があった。 However, the conductive adhesive sheet as described above is often not sufficient in terms of the reworkability, and there are cases where it cannot be reused and re-applied.
以上のとおり、電磁波等を十分に遮蔽可能なレベルの導電性と、被着体が有する段差部等に追従可能なレベルの柔軟性と、リワーク性とを両立した導電性粘着シートは、未だ見出されていなかった。 As described above, a conductive adhesive sheet that has both a level of conductivity that can sufficiently shield electromagnetic waves and the like, a level of flexibility that can follow the stepped portion, etc. of the adherend, and reworkability has not yet been found. It was not put out.
本発明が解決しようとする課題は、電磁波等を十分に遮蔽可能なレベルの導電性と、被着体が有する段差部等に追従可能なレベルの柔軟性と、リワーク性とを両立した導電性粘着シートを提供することにある。 The problem to be solved by the present invention is a conductivity that has both a level of conductivity that can sufficiently shield electromagnetic waves and the like, a level of flexibility that can follow the stepped portion, etc. of the adherend, and reworkability. It is to provide an adhesive sheet.
本発明においては、導電性基材の少なくとも片面に、導電性粘着剤層を有する導電性粘着シートのうち、前記導電性基材が、湿式ポリエステル系不織布基材に、無電解メッキ処理を含むメッキ処理を施すことによって得られたものであり、
前記導電性粘着剤層が、前記導電性粘着剤層全体に対して導電性粒子を３質量％〜５０質量％含有するものである導電性粘着シートを使用することによって、上記課題を解決した。In the present invention, among the conductive pressure-sensitive adhesive sheets having a conductive pressure-sensitive adhesive layer on at least one side of the conductive base material, the conductive base material is plated with a wet polyester nonwoven fabric base material including an electroless plating treatment. Obtained by processing,
The said subject was solved by using the conductive adhesive sheet in which the said conductive adhesive layer contains 3 mass%-50 mass% of electroconductive particles with respect to the said whole conductive adhesive layer.
本発明の導電性粘着シートは、電磁波等を十分に遮蔽可能なレベルの導電性と、被着体が有する微細な凹凸等に由来した段差部等に追従可能なレベルの柔軟性と、リワーク性とを両立でき、被着体に対する優れた接着力を有することから、例えば電子機器等の製造に使用できる電磁波シールドシート、静電気の帯電を防止するための接地固定用粘着シート等に好適に使用することができる。 The conductive pressure-sensitive adhesive sheet of the present invention has a level of conductivity that can sufficiently shield electromagnetic waves, etc., a level of flexibility that can follow stepped portions and the like derived from fine irregularities of the adherend, and reworkability Since it has excellent adhesion to adherends, it is suitable for use in, for example, electromagnetic wave shielding sheets that can be used in the manufacture of electronic devices and the like, adhesive sheets for grounding fixing to prevent static charge, etc. be able to.
本発明の導電性粘着シートは、導電性基材の少なくとも片面に、導電性粘着剤層を有する導電性粘着シートのうち、前記導電性基材が、湿式ポリエステル系不織布基材に、無電解メッキ処理を含むメッキ処理を施すことによって得られたものであり、前記導電性粘着剤層が、前記導電性粘着剤層全体に対して導電性粒子を３質量％〜５０質量％含有するものであることを特徴とするものである。 The conductive pressure-sensitive adhesive sheet of the present invention is a conductive pressure-sensitive adhesive sheet having a conductive pressure-sensitive adhesive layer on at least one surface of a conductive base material. The conductive adhesive layer contains 3% by mass to 50% by mass of conductive particles with respect to the entire conductive adhesive layer. It is characterized by this.
本発明でいう「シート」とは、少なくとも一層の導電性粘着剤層を導電性基材の少なくとも片面に有する形態を意味する。また、前記シートは、例えば、枚葉、ロール状、薄板状、帯状（テープ状）等の製品形態すべてを含む。 The “sheet” in the present invention means a form having at least one conductive pressure-sensitive adhesive layer on at least one surface of a conductive substrate. Moreover, the said sheet | seat contains all the product forms, such as a sheet | seat, roll shape, thin plate shape, and strip | belt shape (tape shape), for example.
本発明の導電性粘着シートの構成としては、例えば導電性基材の片面に前記導電性粘着剤層を単層または複数層有する構成、前記導電性基材の両面に前記導電性粘着剤層をそれぞれ単層または複層有する構成が挙げられる。 As a structure of the conductive adhesive sheet of the present invention, for example, a structure having a single layer or a plurality of layers of the conductive adhesive layer on one side of the conductive substrate, the conductive adhesive layer on both sides of the conductive substrate. The structure which has a single layer or multiple layers, respectively is mentioned.
本発明の導電性粘着シートとしては、必要に応じて前記導電性基材及び導電性粘着剤層以外の他の層を有していてもよい。 As a conductive adhesive sheet of this invention, you may have other layers other than the said conductive base material and a conductive adhesive layer as needed.
前記導電性粘着シートとしては、１００μｍ以下の総厚さを有するものを使用することが好ましく、６０μm以下の総厚さを有するものを使用することがより好ましく、４０μｍ以下の総厚さを有するものを使用することが、優れた柔軟性、導電性及び接着性を維持し、かつ、電子機器等の薄型化に貢献できるためさらに好ましい。 The conductive adhesive sheet preferably has a total thickness of 100 μm or less, more preferably has a total thickness of 60 μm or less, and has a total thickness of 40 μm or less. Is more preferable because it can maintain excellent flexibility, conductivity and adhesiveness, and contribute to thinning of electronic devices and the like.
また、前記導電性粘着シートの総厚さの下限としては、５μｍ以上であることが好ましい。なお、前記総厚さは、剥離フィルムを含まない導電性粘着シート自体の厚さを指す。 Moreover, as a minimum of the total thickness of the said electroconductive adhesive sheet, it is preferable that it is 5 micrometers or more. In addition, the said total thickness points out the thickness of electroconductive adhesive sheet itself which does not contain a peeling film.
本発明の導電性粘着シートを構成する導電性基材としては、湿式のポリエステル系不織布基材に、無電解メッキ処理を含むメッキ処理を施すことによって得られたものを使用することができる。 As the conductive substrate constituting the conductive pressure-sensitive adhesive sheet of the present invention, one obtained by subjecting a wet polyester nonwoven fabric substrate to plating treatment including electroless plating treatment can be used.
前記導電性基材としては、例えば６μｍ〜５０μｍの厚さを有するものを使用することが好ましく、１０μｍ〜３０μｍの厚さを有するものを使用することがより好ましい。 As said electroconductive base material, it is preferable to use what has a thickness of 6 micrometers-50 micrometers, for example, and it is more preferable to use what has a thickness of 10 micrometers-30 micrometers.
前記導電性基材としては、そのＭＤ（流れ）方向の引張強度が３Ｎ／２０ｍｍ〜３５Ｎ／２０ｍｍであるものを使用することが好ましく、５Ｎ／２０ｍｍ〜３０Ｎ／２０ｍｍであるものを使用することがより好ましく、１０Ｎ／２０ｍｍ〜２７Ｎ／２０ｍｍであるものを使用することがさらに好ましい。 As the conductive substrate, one having a tensile strength in the MD (flow) direction of 3 N / 20 mm to 35 N / 20 mm is preferably used, and one having a tensile strength of 5 N / 20 mm to 30 N / 20 mm is used. More preferably, it is more preferable to use the one of 10 N / 20 mm to 27 N / 20 mm.
また、前記導電性基材としては、そのＴＤ（幅）方向の引張強度が０．５Ｎ／２０ｍｍ〜３５Ｎ／２０ｍｍであるものを使用することが好ましく、３Ｎ／２０ｍｍ〜３０Ｎ／２０ｍｍであるものを使用することがより好ましく、１０Ｎ／２０ｍｍ〜２７Ｎ／２０ｍｍであるものを使用することがさらに好ましい。 Moreover, as said electroconductive base material, it is preferable to use that whose tensile strength of the TD (width) direction is 0.5N / 20mm-35N / 20mm, and what is 3N / 20mm-30N / 20mm. More preferably, it is more preferable to use what is 10N / 20mm-27N / 20mm.
前記範囲のＭＤ（流れ）方向及びＴＤ（幅）方向の引張強度を有する導電性基材を使用することによって、リワーク（剥離）する際に導電性粘着シートの千切れを引き起こしにくく優れたリワーク性を維持でき、かつ、導電性基材と導電性粘着剤層との良好な密着性を備えた導電性粘着シートを得ることができる。 By using a conductive base material having a tensile strength in the MD (flow) direction and TD (width) direction within the above range, the reworkability (exfoliation) makes it difficult to cause the conductive pressure-sensitive adhesive sheet to be shredded and has excellent reworkability. Can be maintained, and a conductive pressure-sensitive adhesive sheet having good adhesion between the conductive substrate and the conductive pressure-sensitive adhesive layer can be obtained.
前記導電性基材としては、その［ＭＤ方向の引張強度／ＴＤ方向の引張強度］が０．７〜１．３の範囲であるものを使用することが、リワーク（剥離）する際に導電性粘着シートの千切れを引き起こしにくく優れたリワーク性を維持することができるため好ましい。なお、前記引張強度はＪＩＳ Ｚ０２３７−２０１０にしたがい、３００ｍｍ／ｍｉｎの速度で引っ張ることによって測定された値を指す。 As the conductive base material, a material having a [MD direction tensile strength / TD direction tensile strength] in the range of 0.7 to 1.3 is used when reworking (peeling). It is preferable because it is difficult to cause tearing of the pressure-sensitive adhesive sheet and can maintain excellent reworkability. In addition, the said tensile strength points out the value measured by pulling at a speed | rate of 300 mm / min according to JISZ0237-2010.
また、前記導電性基材としては、０．５Ω／２５ｍｍ×２５ｍｍ以下の表面抵抗値（ｘ軸方向，ｙ軸方向）を有するものを使用することが好ましく、０．１Ω／２５ｍｍ×２５ｍｍ以下の表面抵抗値（ｘ軸方向，ｙ軸方向）を有するものを使用することがより好ましく、０．０５Ω／２５ｍｍ×２５ｍｍ以下の表面抵抗値（ｘ軸方向，ｙ軸方向）を有するものを使用することがさらに好ましく、０．０１Ω／２５ｍｍ×２５ｍｍ以下の表面抵抗値（ｘ，ｙ）を有するものを使用することが、より一層優れた導電性を付与するうえで特に好ましい。 Moreover, as said electroconductive base material, it is preferable to use what has a surface resistance value (x-axis direction, y-axis direction) of 0.5 Ω / 25 mm × 25 mm or less, and 0.1 Ω / 25 mm × 25 mm or less. It is more preferable to use one having a surface resistance value (x-axis direction, y-axis direction), and one having a surface resistance value (x-axis direction, y-axis direction) of 0.05Ω / 25 mm × 25 mm or less is used. It is more preferable to use a material having a surface resistance value (x, y) of 0.01Ω / 25 mm × 25 mm or less, in order to give even more excellent conductivity.
また、前記導電性基材としては、０．１Ω／２５ｍｍ×２５ｍｍ以下の垂直表面抵抗値（ｚ軸方向）を有するものを使用することが好ましく、０．０５Ω／２５ｍｍ×２５ｍｍ以下の垂直表面抵抗値（ｚ軸方向）を有するものを使用することがより好ましく、０．０３Ω／２５ｍｍ×２５ｍｍ以下の垂直表面抵抗値（ｚ軸方向）を有するものを使用することが好ましく、０．０１Ω／２５ｍｍ×２５ｍｍ以下の垂直表面抵抗値（ｚ軸方向）を有するものを使用することが、より一層優れた導電性を付与するうえで特に好ましい。なお、前記表面抵抗値（ｘ軸方向，ｙ軸方向）及び垂直表面抵抗値（ｚ軸方向）の測定方法は実施例に記載した方法で測定した値を指す。 The conductive substrate preferably has a vertical surface resistance value (z-axis direction) of 0.1Ω / 25 mm × 25 mm or less, and has a vertical surface resistance of 0.05Ω / 25 mm × 25 mm or less. It is more preferable to use a material having a value (z-axis direction), and it is preferable to use a material having a vertical surface resistance value (z-axis direction) of 0.03Ω / 25 mm × 25 mm or less, and 0.01Ω / 25 mm. It is particularly preferable to use one having a vertical surface resistance value (z-axis direction) of × 25 mm or less in order to impart even more excellent conductivity. In addition, the measuring method of the said surface resistance value (x-axis direction, y-axis direction) and a perpendicular | vertical surface resistance value (z-axis direction) points out the value measured by the method described in the Example.
前記導電性基材を製造する際には、湿式のポリエステル系不織布基材を使用する。前記特定の不織布基材を使用することによって、メッキ処理により形成されたメッキ層の剥がれを防止でき、より一層優れたリワーク性を備えた導電性粘着シートを得ることができる。 When manufacturing the said electroconductive base material, a wet polyester nonwoven fabric base material is used. By using the specific nonwoven fabric base material, it is possible to prevent peeling of the plating layer formed by the plating treatment, and it is possible to obtain a conductive pressure-sensitive adhesive sheet having further excellent reworkability.
前記湿式ポリエステル系不織布基材としては、水等に分散されたポリエステル繊維を抄紙することによって得られたものを使用することができる。 As the wet polyester non-woven fabric substrate, those obtained by paper-making polyester fibers dispersed in water or the like can be used.
前記ポリエステル繊維としては、例えば２μｍ〜１０μｍの直径を有する繊維を使用することが好ましく、３μｍ〜８μｍの直径を有する繊維を使用することがより好ましい。 As said polyester fiber, it is preferable to use the fiber which has a diameter of 2 micrometers-10 micrometers, for example, and it is more preferable to use the fiber which has a diameter of 3 micrometers-8 micrometers.
前記抄紙方法としては、特に限定されないが、例えば円網抄紙機、短網抄紙機、長網抄紙機、傾斜短網抄紙機を用いる方法が挙げられる。 The paper making method is not particularly limited, and examples thereof include a method using a circular paper machine, a short paper machine, a long paper machine, and an inclined short paper machine.
前記湿式ポリエステル系不織布基材としては、前記方法で抄紙した後、ポリエステル繊維間を結着させることを目的として、加熱等されたものを使用することが好ましい。 As the wet polyester-based non-woven fabric substrate, it is preferable to use a heated one for the purpose of binding the polyester fibers after paper making by the above method.
前記湿式ポリエステル系不織布基材としては、より一層優れた柔軟性と強度とを両立するうえで、２ｇ／ｍ２〜２０ｇ／ｍ２の範囲の坪量を有するものを使用することが好ましく、４ｇ／ｍ２〜１６ｇ／ｍ２の範囲の坪量を有するものを使用することがより好ましく、６ｇ／ｍ２〜１５ｇ／ｍ２の範囲の坪量を有するものを使用することが、薄型でリワーク性に優れた導電性粘着シートを得るうえでさらに好ましい。The wet polyester nonwoven fabric base material preferably has a basis weight in the range of 2 g / m 2 to 20 g / m 2 in order to achieve both more excellent flexibility and strength. / m is more preferable to use those having a basis weight of 2 range ～16G / m 2, is possible to use those having a basis weight in the range of 6 g /
前記湿式ポリエステル不織布基材としては、５μ〜５０μｍの厚さを有するものを使用することが好ましく、１０μｍ〜３０μｍの厚さを有するものを使用することがより好ましく、１４μｍ〜２０μｍの厚さを有するものを使用することが特に好ましい。 As the wet polyester nonwoven fabric substrate, one having a thickness of 5 μm to 50 μm is preferably used, more preferably one having a thickness of 10 μm to 30 μm, and more preferably 14 μm to 20 μm. It is particularly preferred to use one.
前記湿式ポリエステル系不織布基材としては、そのＭＤ（流れ）方向の引張強度が２Ｎ／２０ｍｍ〜３０Ｎ／２０ｍｍであるものを使用することが好ましく、５Ｎ／２０ｍｍ〜２８Ｎ／２０ｍｍであるものを使用することがより好ましく、１０Ｎ／２０ｍｍ〜２５Ｎ／２０ｍｍであるものを使用することがさらに好ましい。 The wet polyester nonwoven fabric base material preferably has a MD (flow) direction tensile strength of 2 N / 20 mm to 30 N / 20 mm, preferably 5 N / 20 mm to 28 N / 20 mm. It is more preferable to use a material having a thickness of 10 N / 20 mm to 25 N / 20 mm.
また、前記湿式ポリエステル系不織布基材としては、そのＴＤ（幅）方向の引張強度が０．３Ｎ／２０ｍｍ〜３０Ｎ／２０ｍｍであるものを使用することが好ましく、２Ｎ／２０ｍｍ〜２７Ｎ／２０ｍｍであるものを使用することがより好ましく、９Ｎ／２０ｍｍ〜２５Ｎ／２０ｍｍであるものを使用することがさらに好ましい。なお、前記引張強度はＪＩＳ Ｚ０２３７−２０１０にしたがい、３００ｍｍ／ｍｉｎの速度で引っ張ることによって測定された値を指す。 The wet polyester nonwoven fabric base material preferably has a tensile strength in the TD (width) direction of 0.3 N / 20 mm to 30 N / 20 mm, and preferably 2 N / 20 mm to 27 N / 20 mm. It is more preferable to use a thing, and it is still more preferable to use what is 9N / 20mm-25N / 20mm. In addition, the said tensile strength points out the value measured by pulling at a speed | rate of 300 mm / min according to JISZ0237-2010.
前記導電性基材は、前記湿式ポリエステル系不織布基材に、無電解メッキ処理を含むメッキ処理を施すことによって製造することができる。ここで、「無電解メッキ処理を含むメッキ処理」とは、無電解メッキ処理を１回または複数回行う処理、前記無電解メッキ処理後に電解メッキ処理を１回または複数回行う処理、及び、電解メッキ処理を１回または複数回行った後に無電解メッキ処理を１回または複数回行う処理を指す。本発明では、無電解メッキ処理を施した後に、さらに無電解メッキ処理または電解メッキ処理を施すことが好ましく、無電解メッキ処理を施した後に、さらに電解メッキ処理を施すことがより好ましい。 The conductive substrate can be produced by subjecting the wet polyester nonwoven fabric substrate to a plating treatment including an electroless plating treatment. Here, “plating process including electroless plating process” means a process of performing electroless plating process once or a plurality of times, a process of performing electroplating process once or a plurality of times after the electroless plating process, and electrolysis This refers to a process in which the electroless plating process is performed once or a plurality of times after the plating process is performed once or a plurality of times. In the present invention, it is preferable to further perform an electroless plating process or an electrolytic plating process after performing the electroless plating process, and it is more preferable to perform an electrolytic plating process after performing the electroless plating process.
前記無電解メッキ処理法としては、例えばパラジウムなどの触媒を含む液や、金属イオンと還元剤とを含有する無電解メッキ液に、前記湿式不飽和ポリエステル系不織布基材を浸漬することによって、前記不織布基材の表面に金属皮膜を形成する方法が挙げられる。 As the electroless plating treatment method, for example, by immersing the wet unsaturated polyester nonwoven fabric substrate in a liquid containing a catalyst such as palladium, or an electroless plating liquid containing a metal ion and a reducing agent, The method of forming a metal film on the surface of a nonwoven fabric base material is mentioned.
また、前記無電解メッキ処理をする際には、前記した工程のほかに、前記湿式ポリエステル系不織布基材を洗浄する工程、前記触媒を活性化する工程、湿式ポリエステル系不織布基材及びメッキ処理されたものを水洗または乾燥する工程を経てもよい。 Further, when performing the electroless plating treatment, in addition to the steps described above, the step of washing the wet polyester nonwoven fabric substrate, the step of activating the catalyst, the wet polyester nonwoven fabric substrate and the plating treatment are performed. You may pass through the process of washing or drying a thing.
前記無電解メッキ処理する好ましい方法としては、前記湿式ポリエステル系不織布基材を洗浄し、水洗した後、前記湿式ポリエステル系不織布基材に触媒を付与し、水洗し、前記触媒を活性化し、水洗し、湿式ポリエステル系不織布基材を無電解メッキ液に浸漬し、水洗し乾燥する方法が挙げられる。 As a preferred method for the electroless plating treatment, the wet polyester nonwoven fabric substrate is washed and washed with water, then a catalyst is applied to the wet polyester nonwoven fabric substrate, washed with water, the catalyst is activated, and washed with water. The wet polyester type nonwoven fabric base material is immersed in an electroless plating solution, washed with water and dried.
前記無電解メッキ液に含まれる金属イオンとしては、例えば銅、ニッケル、銀、白金、アルミニウム等のイオン挙げられ、銅またはニッケルの少なくとも１種のイオンを使用することが、より一層優れた導電性と低コストとを両立するうえで好ましく、銅イオンを使用することが、より一層優れた密着性を付与するうえでより好ましい。 Examples of the metal ions contained in the electroless plating solution include ions such as copper, nickel, silver, platinum, and aluminum, and the use of at least one ion of copper or nickel further improves conductivity. In view of achieving both low cost and low cost, it is more preferable to use copper ions to provide even better adhesion.
前記金属イオンは、前記無電解メッキ液に対して、０．００１モル／ｌ〜０．２モル／ｌ含まれることが好ましい。 The metal ions are preferably contained in an amount of 0.001 mol / l to 0.2 mol / l with respect to the electroless plating solution.
前記金属イオンは、硫酸銅、硫酸ニッケル、塩化ニッケル、塩化パラジウム、塩化銀、硝酸銀及びこれらの混合物に由来するものであることが好ましく、硫酸銅、硫酸ニッケル、塩化ニッケルを使用することが、より一層優れた導電性と低コストとを両立するうえで好適な銅またはニッケルイオンを存在させるうえで好ましい。 The metal ions are preferably derived from copper sulfate, nickel sulfate, nickel chloride, palladium chloride, silver chloride, silver nitrate and mixtures thereof, and more preferably using copper sulfate, nickel sulfate, nickel chloride, It is preferable for the presence of copper or nickel ions suitable for achieving both excellent conductivity and low cost.
前記無電解メッキ液に含有されていてもよい還元剤としては、例えば次亜燐酸ナトリム、水素化ホウ素ナトリウム、水素化ホウ素カリウム、ロッシェル塩、ジメチルアミンボラン、ジエチルアミンボラン、ホルマリン、ヒドラジン化合物としては、水和ヒドラジン、塩酸ヒドラジン、硫酸ヒドラジン、メチルヒドラジン、１，２−ジメチルヒドラジン、アセトヒドラジン、フェニルヒドラジン等がハイドロキノン等を使用することができ、次亜燐酸ナトリムやホルマリンを使用することが好ましい。 Examples of the reducing agent that may be contained in the electroless plating solution include sodium hypophosphite, sodium borohydride, potassium borohydride, Rochelle salt, dimethylamine borane, diethylamine borane, formalin, and hydrazine compounds. Hydrated hydrazine, hydrazine hydrochloride, hydrazine sulfate, methyl hydrazine, 1,2-dimethyl hydrazine, acetohydrazine, phenyl hydrazine and the like can use hydroquinone and the like, preferably sodium hypophosphite and formalin.
前記還元剤は、前記無電解メッキ液に対して、０．００１モル／ｌ〜０．４モル／ｌ含まれることが好ましい。 The reducing agent is preferably contained in an amount of 0.001 mol / l to 0.4 mol / l with respect to the electroless plating solution.
前記無電解メッキ液としては、前記成分の他に、補助成分として、錯化剤、ｐＨ調整剤、緩衝剤、メッキ促進剤、安定剤等を含有するものを使用することができる。 As said electroless-plating liquid, what contains a complexing agent, a pH adjuster, a buffering agent, a plating accelerator, a stabilizer, etc. can be used as an auxiliary component other than the said component.
前記錯化剤としては、例えばクエン酸ナトリウム、クエン酸カリウム、ロッシェル塩等の有機酸塩、チオグリコール酸、アンモニア、トリエタノールアミン、グリシン、エチレンジアミン、エチレンジアミン２酢酸塩、ｏ−アミノフェノール、ピリジン等を使用することができ、クエン酸ナトリムを使用することが好ましい。 Examples of the complexing agent include organic acid salts such as sodium citrate, potassium citrate, and Rochelle salt, thioglycolic acid, ammonia, triethanolamine, glycine, ethylenediamine, ethylenediamine diacetate, o-aminophenol, pyridine, and the like. It is preferable to use sodium citrate.
前記錯化剤は、前記無電解メッキ液に対して、０．００１モル／ｌ〜４．０モル／ｌ含まれることが好ましい。 The complexing agent is preferably contained in an amount of 0.001 mol / l to 4.0 mol / l with respect to the electroless plating solution.
前記ｐＨ調整剤としては、例えば水酸化ナトリウム、水酸化アンモニウム、無機酸、有機酸等を使用することが好ましい。 As the pH adjuster, for example, sodium hydroxide, ammonium hydroxide, inorganic acid, organic acid or the like is preferably used.
前記緩衝剤としては、例えば有機酸、無機酸のアルカリ金属塩、クエン酸ナトリウム、酢酸ナトリウム、塩化アンモニウム、硫酸アンモニウム、オキシカルボン酸、燐酸２水素塩、ホウ酸、炭酸等を使用することが好ましい。 As the buffer, it is preferable to use, for example, an alkali metal salt of an organic acid or an inorganic acid, sodium citrate, sodium acetate, ammonium chloride, ammonium sulfate, oxycarboxylic acid, dihydrogen phosphate, boric acid, carbonic acid, or the like.
前記メッキ促進剤としては、硫化物、フッ化物等を使用することができる。 As the plating accelerator, sulfide, fluoride, or the like can be used.
前記安定剤としては、鉛の塩化物、硫化物、硝化物、２，２−ビピリジン、２−メルカプトベンゾチアゾール、ニコチン酸等を適宜使用することができる。 As the stabilizer, lead chloride, sulfide, nitride, 2,2-bipyridine, 2-mercaptobenzothiazole, nicotinic acid and the like can be appropriately used.
前記無電解メッキ処理法によって前記湿式ポリエステル系不織布基材の表面に積層された、好ましくは銅等の金属は、より一層優れた密着性と導電性とを有し、前記処理に要するコストを低減させるうえで、１ｇ／ｍ２〜２０ｇ／ｍ２の範囲であることが好ましく、３ｇ／ｍ２〜１０ｇ／ｍ２の範囲であることがより好ましく、５ｇ／ｍ２〜８ｇ／ｍ２の範囲であることがさらに好ましい。A metal such as copper, which is laminated on the surface of the wet polyester nonwoven fabric substrate by the electroless plating method, preferably has even better adhesion and conductivity, reducing the cost required for the treatment. upon which, 1 g /
本発明で使用する導電性基材としては、前記したとおり、湿式ポリエステル系不織布基材を無電解金属メッキ処理した後、さらに無電解メッキ処理または電解メッキ処理したものを使用することが好ましく、特に電解メッキ処理したものを使用することが、メッキ層を比較的短時間で安定して形成できることから生産コストの低減ができ、かつ、高強度化とを図ることができるためより好ましい。 As described above, as the conductive base material used in the present invention, it is preferable to use a wet polyester-based nonwoven fabric base material that has been subjected to an electroless metal plating treatment and then subjected to an electroless plating treatment or an electrolytic plating treatment. It is more preferable to use what has been subjected to electroplating because the plating layer can be stably formed in a relatively short time because the production cost can be reduced and the strength can be increased.
前記電解メッキ処理に使用できる電解メッキ液としては、例えばピロリン酸銅、シアン化銅浴、硫酸銅浴等を含む銅メッキ液、ワット浴、塩化浴、スルファミン酸浴等を含むニッケルメッキ液、サージェント浴等を含むクロムメッキ液、または、金、銀、錫、亜鉛等を含むメッキ液を使用することができる。 Examples of the electrolytic plating solution that can be used for the electrolytic plating treatment include copper plating solutions including copper pyrophosphate, copper cyanide bath, copper sulfate bath, nickel plating solutions including watt bath, chloride bath, sulfamic acid bath, and the like. A chromium plating solution containing a bath or the like, or a plating solution containing gold, silver, tin, zinc or the like can be used.
前記導電性基材としては、その最外層がニッケルを含むめっき層であるものを使用することが、保存安定性に優れ、湿式ポリエステル系不織布基材とメッキ層との密着性の点で優れ、かつ、導電性に優れるため好ましい。 As the conductive base material, it is excellent in storage stability that the outermost layer is a plating layer containing nickel, and excellent in terms of adhesion between the wet polyester nonwoven fabric base material and the plating layer, And since it is excellent in electroconductivity, it is preferable.
前記最外層は、ニッケルを１ｇ／ｍ２〜１０ｇ／ｍ２含むことが好ましく、２ｇ／ｍ２〜８ｇ／ｍ２含むことがより好ましく、２．５ｇ／ｍ２〜６ｇ／ｍ２含むことが、前記優れた保存安定性と密着性と導電性とを両立するうえでさらに好ましい。The outermost layer preferably contains 1g / m 2 ~10g /
前記導電性基材の好ましい態様としては、例えば、湿式のポリエステル系不織布基材に、無電解銅メッキ処理、及び、電解ニッケルメッキ処理が順に施された導電性基材、湿式のポリエステル系不織布基材に、無電解銅メッキ処理、電解銅メッキ処理及び電解ニッケルメッキ処理が順に施された導電性基材が挙げられる。 As a preferable aspect of the conductive base material, for example, a wet base polyester non-woven base material, a non-electrolytic copper plating process, and a conductive base material subjected to an electrolytic nickel plating process in order, a wet base polyester non-woven base Examples of the material include a conductive base material in which an electroless copper plating process, an electrolytic copper plating process, and an electrolytic nickel plating process are sequentially performed.
次に、本発明の導電性粘着シートを構成する導電性粘着剤層について説明する。 Next, the electroconductive adhesive layer which comprises the electroconductive adhesive sheet of this invention is demonstrated.
前記導電性粘着剤層は、前記導電性粘着剤層全体に対して導電性粒子を３質量％〜５０質量％含有するものである。かかる導電性粘着剤層を有する導電性粘着シートは、優れた導電性を有する。 The conductive pressure-sensitive adhesive layer contains 3% by mass to 50% by mass of conductive particles with respect to the entire conductive pressure-sensitive adhesive layer. A conductive pressure-sensitive adhesive sheet having such a conductive pressure-sensitive adhesive layer has excellent conductivity.
前記導電性粘着剤層としては、前記導電性粘着剤層全体に対して導電性粒子を５質量％〜５０質量％含有するものを使用することが好ましく、１０質量％〜５０質量％含有するものを使用することがより好ましく、１５質量％〜４５質量％含有するものを使用することが、より一層優れた導電性と、被着体が有する段差部等に追従可能なレベルの柔軟性と、リワーク性とを発現できるため好ましい。 The conductive adhesive layer preferably contains 5% to 50% by mass of conductive particles with respect to the entire conductive adhesive layer, and preferably contains 10% to 50% by mass. It is more preferable to use a material containing 15% by mass to 45% by mass, more excellent electrical conductivity, and a level of flexibility that can follow the stepped portion and the like of the adherend, Since reworkability can be expressed, it is preferable.
前記導電性粘着剤層としては、３μｍ〜２５μｍの厚さであるものを使用することが好ましく、５μｍ〜２０μｍの厚さであるものを使用することがより好ましく、７μｍ〜１８μｍの厚さのであるものを使用することが、より一層優れた接着性と、薄型化とを両立した導電性粘着シートを得ることができる。 The conductive adhesive layer preferably has a thickness of 3 μm to 25 μm, more preferably has a thickness of 5 μm to 20 μm, and preferably has a thickness of 7 μm to 18 μm. Use of a material can provide a conductive pressure-sensitive adhesive sheet that achieves both excellent adhesion and thinning.
前記導電性粘着剤層としては、導電性粒子と粘着剤成分とを含有する粘着剤組成物を用いることによって形成することができる。 The conductive pressure-sensitive adhesive layer can be formed by using a pressure-sensitive adhesive composition containing conductive particles and a pressure-sensitive adhesive component.
前記導電性粘着剤層に含まれる導電性粒子としては、例えば金、銀、銅、ニッケル、アルミニウム等の金属粒子、カーボン、グラファイト等の導電性樹脂粒子、前記樹脂や中実ガラスビーズや中空ガラスビーズの表面が金属被覆された粒子等を使用することができる。なかでも、前記導電性粒子としては、ニッケル粒子や銅粒子や銀粒子を使用することが、より一層優れた導電性及び接着強さを備え、かつ導電性粘着シートの生産性をより一層向上するうえで好ましい。 Examples of the conductive particles contained in the conductive adhesive layer include metal particles such as gold, silver, copper, nickel, and aluminum, conductive resin particles such as carbon and graphite, the resin, solid glass beads, and hollow glass. For example, particles whose surface is coated with metal can be used. Among them, the use of nickel particles, copper particles, or silver particles as the conductive particles further improves the conductivity and adhesive strength, and further improves the productivity of the conductive adhesive sheet. In addition, it is preferable.
また、前記導電性粒子としては、例えばカーボニル法で製造される粒子表面に多数の針状形状を有する表面針状形状のニッケル粒子や、当該表面針状粒子を平滑化処理して球状粒子としたものや、超高圧旋回水アトマイズ法で製造される銅粒子や銀粒子があげられる。 Moreover, as the conductive particles, for example, surface needle-like nickel particles having a large number of needle-like shapes on the surface of particles produced by the carbonyl method, or the surface needle-like particles are smoothed to obtain spherical particles. And copper particles and silver particles produced by the ultra high pressure swirling water atomization method.
前記導電性粒子のとしては、球状または表面針状形状であるものを使用することが好ましい。前記導電性粒子としては、１〜２のアスペクト比を有するものを使用することが好ましく、１〜１．５のアスペクト比を有するものを使用することがより好ましく、１〜１．２のアスペクト比を有するものを使用することがさらに好ましい。前記アスペクト比は、前記導電性粒子の表面を、走査型電子顕微鏡を用い観察することで測定することができる。 As the conductive particles, those having a spherical shape or a surface needle shape are preferably used. As the conductive particles, it is preferable to use particles having an aspect ratio of 1 to 2, more preferably particles having an aspect ratio of 1 to 1.5, and an aspect ratio of 1 to 1.2. It is more preferable to use one having The aspect ratio can be measured by observing the surface of the conductive particles using a scanning electron microscope.
前記導電性粒子としては、２ｇ／ｃｍ３〜７ｇ／ｃｍ３のタップ密度を有するものを使用することが、導電性粘着剤層を形成する際に沈降や凝集しにくいため好ましく、３ｇ／ｃｍ３〜６ｇ／ｃｍ３のタップ密度を有するものを使用することがより好ましく、４ｇ／ｃｍ３〜５ｇ／ｃｍ３のタップ密度を有するものを使用することがさらに好ましい。As the conductive particles, is possible to use those having a tap density of 2g / cm 3 ~7g / cm 3 , preferably for hard settling and aggregation at the time of forming the conductive pressure sensitive adhesive layer, 3 g / cm 3 it is more preferred to use those having a tap density of to 6 g / cm 3, it is more preferable to use those having a tap density of 4g / cm 3 ~5g / cm 3 .
前記導電性粒子としては、その粒子径ｄ５０が３μｍ〜２０μｍであり、かつ、その粒子径ｄ８５が６μｍ〜４０μｍであるものを使用することが好ましい。 As the conductive particles, particles having a particle diameter d50 of 3 μm to 20 μm and a particle diameter d85 of 6 μm to 40 μm are preferably used.
前記導電性粒子の前記粒子径ｄ５０は、より好ましくは４μｍ〜１５μｍであり、さらに好ましくは５μｍ〜１２μｍであり、特に好ましくは６μｍ〜１０μｍである。 The particle diameter d50 of the conductive particles is more preferably 4 μm to 15 μm, still more preferably 5 μm to 12 μm, and particularly preferably 6 μm to 10 μm.
また、前記導電性粒子の前記粒子径ｄ８５は、より好ましくは８μｍ〜３０μｍであり、さらに好ましくは９μｍ〜２５μｍであり、特に好ましくは１０μｍ〜２０μｍである。なお、導電性粒子を２種以上組み合わせ使用する場合、それらの混合物の平均粒子径ｄ５０及びｄ８５が上記範囲であるものを使用することが好ましい。 The particle diameter d85 of the conductive particles is more preferably 8 μm to 30 μm, still more preferably 9 μm to 25 μm, and particularly preferably 10 μm to 20 μm. In addition, when using 2 or more types of electroconductive particles in combination, it is preferable to use those whose average particle diameters d50 and d85 of the mixture are the said range.
なお、前記粒子径ｄ５０は粒度分布における５０％累積値（メディアン径）を表し、前記粒子径ｄ８５は８５％累積値を表す。具体的には、前記粒子径は、レーザー解析・散乱法によって測定される値である。測定装置としては株式会社島津製作所製レーザー回折式粒度分布測定器ＳＡＬＤ−３０００で測定した値を指す。 The particle diameter d50 represents a 50% cumulative value (median diameter) in the particle size distribution, and the particle diameter d85 represents an 85% cumulative value. Specifically, the particle diameter is a value measured by a laser analysis / scattering method. As a measuring apparatus, the value measured with the laser diffraction type particle size distribution measuring device SALD-3000 by Shimadzu Corporation is pointed out.
前記導電性粒子としては、前記粒子径ｄ５０が前記導電性粘着剤層の厚さの５０％〜１５０％となるものを選択し使用することが好ましく、６０％〜１２０％となるものを選択し使用することがより好ましく、７０％〜１００％となるものを選択し使用することがさらに好ましい。 As the conductive particles, those having a particle diameter d50 of 50% to 150% of the thickness of the conductive pressure-sensitive adhesive layer are preferably selected and used, and those having a particle size of 60% to 120% are selected. It is more preferable to use, and it is still more preferable to select and use what becomes 70% to 100%.
また、前記導電性粒子としては、前記粒子径ｄ８５が前記導電性粘着剤層の厚さの８０％〜２００％となるものを選択し使用することがより好ましく、１００％〜１５０％となるものを選択し使用することがより好ましく、１１０％〜１４０％となるものを選択し使用することがさらに好ましい。 Further, as the conductive particles, it is more preferable to select and use particles having a particle diameter d85 of 80% to 200% of the thickness of the conductive adhesive layer, and 100% to 150%. It is more preferable to select and use, and it is more preferable to select and use the one that is 110% to 140%.
前記粒子径ｄ５０及びｄ８５の導電性粒子を使用することによって、より一層導電性及び接着強さに優れ、かつ導電性粘着シートの生産効率をより一層向上させることができる。 By using the conductive particles having the particle diameters d50 and d85, the conductivity and adhesive strength are further improved, and the production efficiency of the conductive adhesive sheet can be further improved.
前記導電性粒子は、前記導電性粘着剤層に含まれる粘着剤成分（固形分）１００質量部に対して５質量部〜１００質量部の範囲で使用することが好ましく、１０質量部〜１００質量部の範囲で使用することがより好ましく、２０質量部〜８０質量部の範囲で使用することが、より一層導電性及び接着強さに優れ、かつ導電性粘着シートの生産効率をより一層向上させることができるため特に好ましい。具体的には、前記導電性粒子は、前記導電性粘着剤層に含まれるアクリル系重合体（固形分）１００質量部に対して５質量部〜１００質量部の範囲で使用することが好ましく、１０質量部〜１００質量部の範囲で使用することがより好ましく、２０質量部〜８０質量部の範囲で使用することが、より一層導電性及び接着強さに優れ、かつ導電性粘着シートの生産効率をより一層向上させることができるため特に好ましい。 The conductive particles are preferably used in the range of 5 to 100 parts by mass with respect to 100 parts by mass of the adhesive component (solid content) contained in the conductive adhesive layer. More preferably, it is used in the range of 20 parts by weight to 80 parts by weight, and the conductivity and adhesive strength are further improved, and the production efficiency of the conductive adhesive sheet is further improved. It is particularly preferable because it can be used. Specifically, the conductive particles are preferably used in a range of 5 to 100 parts by mass with respect to 100 parts by mass of the acrylic polymer (solid content) contained in the conductive adhesive layer. It is more preferable to use in the range of 10 parts by mass to 100 parts by mass, and use in the range of 20 parts by mass to 80 parts by mass further improves the conductivity and adhesive strength, and produces a conductive pressure-sensitive adhesive sheet. It is particularly preferable because the efficiency can be further improved.
前記導電性粒子と前記粘着剤成分とを混合する方法としては、例えば、導電性物質と、粘着剤成分であるアクリル系重合体等の粘着剤成分と、前記添加剤等とを混合する方法が挙げられる。前記アクリル系重合体等の粘着剤成分と溶媒と、必要に応じて添加剤とは、予め混合されていてもよい。前記混合には、ディゾルバー、バタフライミキサー、ＢＤＭ２軸ミキサー、プラネタリーミキサー等の分散混合機を使用することができる。なかでも前記混合の際の粘度の上昇を抑制できる中程度のシェアをかけることが可能なディゾルバー、バタフライミキサーを使用することが好ましい。 As a method of mixing the conductive particles and the pressure-sensitive adhesive component, for example, a method of mixing a conductive material, a pressure-sensitive adhesive component such as an acrylic polymer that is a pressure-sensitive adhesive component, and the additive or the like. Can be mentioned. The pressure-sensitive adhesive component such as the acrylic polymer, a solvent, and, if necessary, an additive may be mixed in advance. For the mixing, a dispersion mixer such as a dissolver, a butterfly mixer, a BDM biaxial mixer, or a planetary mixer can be used. Among them, it is preferable to use a dissolver and a butterfly mixer capable of applying a medium share that can suppress an increase in viscosity during the mixing.
また、前記導電性粘着剤層を構成する粘着剤成分としては、例えばアクリル系粘着剤組成物、シリコーン系粘着剤組成物、ゴム系粘着剤組成物等を使用することができる。なかでも、前記粘着剤成分としては、導電性粘着シート生産コストの低減と、接着性の更なる向上を図るうえでアクリル系粘着剤組成物を使用することが好ましい。 Moreover, as an adhesive component which comprises the said electroconductive adhesive layer, an acrylic adhesive composition, a silicone type adhesive composition, a rubber-type adhesive composition etc. can be used, for example. Among these, as the pressure-sensitive adhesive component, it is preferable to use an acrylic pressure-sensitive adhesive composition in order to reduce the production cost of the conductive pressure-sensitive adhesive sheet and further improve the adhesiveness.
前記アクリル系粘着剤組成物としては、例えばアクリル系重合体を含有するものを使用することができる。 As said acrylic adhesive composition, what contains an acrylic polymer can be used, for example.
前記アクリル系重合体としては、単量体成分を重合して得られるものを使用することができる。 As the acrylic polymer, those obtained by polymerizing monomer components can be used.
前記単量体成分としては、例えば炭素原子数１〜１４のアルキル基を有する（メタ）アクリレートを含有する単量体成分を使用することができる。 As the monomer component, for example, a monomer component containing (meth) acrylate having an alkyl group having 1 to 14 carbon atoms can be used.
前記炭素原子数１〜１４のアルキル基を有する（メタ）アクリレートとしては、例えば、メチル（メタ）アクリレート、エチル（メタ）アクリレート、ｎ−ブチル（メタ）アクリレート、イソブチル（メタ）アクリレート、ｔ−ブチル（メタ）アクリレート、ｎ−ヘキシル（メタ）アクリレート、ｎ−オクチル（メタ）アクリレート、イソオクチル（メタ）アクリレート、イソノニル（メタ）アクリレート、シクロヘキシル（メタ）アクリレート、２−エチルヘキシル（メタ）アクリレート等を単独または２種以上組み合わせ使用することができる。 Examples of the (meth) acrylate having an alkyl group having 1 to 14 carbon atoms include methyl (meth) acrylate, ethyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl (meth) acrylate, and t-butyl. (Meth) acrylate, n-hexyl (meth) acrylate, n-octyl (meth) acrylate, isooctyl (meth) acrylate, isononyl (meth) acrylate, cyclohexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate or the like alone or Two or more kinds can be used in combination.
なかでも、前記炭素原子数１〜１４のアルキル基を有する（メタ）アクリレートとしては、炭素原子数が４〜１２のアルキル基を有する（メタ）アクリレートを使用することが好ましく、炭素原子数が４〜９の直鎖または分岐したアルキル基を有する（メタ）アクリレートを使用することがより好ましく、ｎ−ブチルアクリレート、２−エチルヘキシルアクリレートを単独または２種を組み合わせ使用することがさらに好ましい。 Especially, as said (meth) acrylate which has a C1-C14 alkyl group, it is preferable to use the (meth) acrylate which has a C4-C12 alkyl group, and a carbon atom number is four. It is more preferable to use (meth) acrylate having a linear or branched alkyl group of ˜9, and it is more preferable to use n-butyl acrylate and 2-ethylhexyl acrylate alone or in combination.
前記炭素原子数１〜１４のアルキル基を有する（メタ）アクリレートは、前記単量体成分の全量に対して８０質量％〜９８．５質量％の範囲で使用することが好ましく、９０質量％〜９８．５質量％の範囲で使用することがより好ましい。 The (meth) acrylate having an alkyl group having 1 to 14 carbon atoms is preferably used in the range of 80% by mass to 98.5% by mass with respect to the total amount of the monomer component, and 90% by mass to It is more preferable to use in the range of 98.5% by mass.
また、本発明に使用するアクリル系重合体を製造する際には、前記単量体成分として極性ビニル単量体を使用することができる。前記極性ビニル単量体としては、水酸基を有するビニル単量体、カルボキシル基を有するビニル単量体、アミド基を有するビニル単量体等を１種または２種以上使用することができる。 Moreover, when manufacturing the acrylic polymer used for this invention, a polar vinyl monomer can be used as said monomer component. As the polar vinyl monomer, one or more vinyl monomers having a hydroxyl group, vinyl monomers having a carboxyl group, vinyl monomers having an amide group, and the like can be used.
カルボキシル基を有するビニル単量体としては、アクリル酸、メタクリル酸、イタコン酸、マレイン酸、（メタ）アクリル酸２量体、クロトン酸、エチレンオキサイド変性琥珀酸アクリレート等を使用でき、なかでもアクリル酸またはメタクリル酸を使用することが好ましく、アクリル酸を使用することがより好ましい。 As vinyl monomers having a carboxyl group, acrylic acid, methacrylic acid, itaconic acid, maleic acid, (meth) acrylic acid dimer, crotonic acid, ethylene oxide-modified succinic acid acrylate, etc. can be used, among which acrylic acid Alternatively, methacrylic acid is preferably used, and acrylic acid is more preferably used.
前記カルボキシル基を有するビニル単量体としては、前記単量体成分の全量に対して１質量％〜１０質量％の範囲で使用することが好ましく、１．５質量％〜６質量％であることがより好ましく、２質量％〜４質量％であることが、被着体を構成する金属面に対する初期接着強さに優れ、かつ、導電性粘着テープを高温高湿下に保存等した場合であっても被着体に対する優れた接着強さを発現できるためさらに好ましい。また、前記カルボキシル基を有するビニル単量体として好ましいアクリル酸は、前記単量体成分の全量に対して１質量％〜６質量％の範囲で使用することが、被着体に対するより一層優れた濡れ性と接着強さとを両立できるため好ましい。 The vinyl monomer having a carboxyl group is preferably used in the range of 1% by mass to 10% by mass with respect to the total amount of the monomer components, and is 1.5% by mass to 6% by mass. More preferably, the content is 2% by mass to 4% by mass when the initial adhesive strength to the metal surface constituting the adherend is excellent and the conductive adhesive tape is stored under high temperature and high humidity. However, it is more preferable because excellent adhesion strength to the adherend can be expressed. Further, acrylic acid preferable as the vinyl monomer having a carboxyl group is more excellent for the adherend when used in the range of 1% by mass to 6% by mass with respect to the total amount of the monomer components. This is preferable because both wettability and adhesive strength can be achieved.
前記水酸基を有するビニル単量体としては、例えば、２−ヒドロキシエチル（メタ）アクリレート、２−ヒドロキシプロピル（メタ）アクリレート、４−ヒドロキシブチル（メタ）アクリレート、６−ヒドロキシヘキシル（メタ）アクリレート等の水酸基を有する（メタ）アクリレートを使用することができる。 Examples of the vinyl monomer having a hydroxyl group include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, and 6-hydroxyhexyl (meth) acrylate. A (meth) acrylate having a hydroxyl group can be used.
前記アミド基を有するビニル単量体としては、例えばＮ−ビニルピロリドン、Ｎ−ビニルカプロラクタム、アクリロイルモルホリン、アクリルアミド、Ｎ，Ｎ−ジメチルアクリルアミド等を使用することができる。 As the vinyl monomer having an amide group, for example, N-vinylpyrrolidone, N-vinylcaprolactam, acryloylmorpholine, acrylamide, N, N-dimethylacrylamide and the like can be used.
その他のビニル単量体としては、例えば酢酸ビニル、エチレンオキサイド変性琥珀酸アクリレート、２−アクリルアミド−２−メチルプロパンスルフォン酸等のスルホン酸基含有モノマー、２−メトキシエチル（メタ）アクリレート、２−フェノキシエチル（メタ）アクリレート等の末端アルコキシ変性（メタ）アクリレート等を使用することができる。 Examples of other vinyl monomers include sulfonic acid group-containing monomers such as vinyl acetate, ethylene oxide-modified succinic acid acrylate, 2-acrylamido-2-methylpropane sulfonic acid, 2-methoxyethyl (meth) acrylate, and 2-phenoxy. Terminal alkoxy-modified (meth) acrylates such as ethyl (meth) acrylate can be used.
前記極性ビニル単量体は、前記単量体成分の全量に対して０．２質量％〜１５質量％の範囲で使用することが好ましく、０．４質量％〜１０質量％の範囲で使用することがより好ましく、０．５質量％〜６質量％の範囲で使用することが、接着強さを好適な範囲に調整しやすいためさらに好ましい。 The polar vinyl monomer is preferably used in a range of 0.2% by mass to 15% by mass with respect to the total amount of the monomer components, and is used in a range of 0.4% by mass to 10% by mass. It is more preferable to use in the range of 0.5% by mass to 6% by mass because it is easy to adjust the adhesive strength to a suitable range.
前記アクリル系重合体は、前記した単量体成分を、溶液重合法、塊状重合法、懸濁重合法、乳化重合法など公知の方法で重合させることによって製造することができ、なかでも生産コストの低減と生産効率の向上とを図るうえで、溶液重合法を採用することが好ましい。 The acrylic polymer can be produced by polymerizing the above monomer components by a known method such as a solution polymerization method, a bulk polymerization method, a suspension polymerization method, an emulsion polymerization method, and the production cost among others. It is preferable to employ a solution polymerization method in order to reduce the amount and improve the production efficiency.
前記方法で得られたアクリル系重合体としては、３０万〜１５０万の重量平均分子量を有するものを使用することが好ましく、５０万〜１２０万の重量平均分子量を有するものを使用することがより好ましい。 As the acrylic polymer obtained by the above method, those having a weight average molecular weight of 300,000 to 1,500,000 are preferably used, and those having a weight average molecular weight of 500,000 to 1,200,000 are more preferably used. preferable.
前記導電性粘着剤層は、より一層凝集力を高め、より一層接着性に優れた効果を奏するうえで、３次元架橋構造を形成していることが好ましい。 The conductive pressure-sensitive adhesive layer preferably has a three-dimensional cross-linked structure in order to further enhance the cohesive force and to further improve the adhesion.
前記架橋の程度は、その指標として、前記アクリル系重合体の良溶媒であるトルエンに２４時間浸漬した後の不溶分で表されるゲル分率を用いることで認識することができる。前記導電性粘着剤層としては、そのゲル分率が２５質量％〜６５質量％であるものを使用することが好ましく、３５質量％〜６０質量％であるものを使用することがより好ましく、４０質量％〜５５質量％であるものを使用することがせん断方向の凝集力及び耐剥がれ性をより良好にすることができるためさらに好ましい。 The degree of cross-linking can be recognized by using a gel fraction represented by an insoluble content after being immersed in toluene, which is a good solvent for the acrylic polymer, for 24 hours. The conductive adhesive layer preferably has a gel fraction of 25% to 65% by weight, more preferably 35% to 60% by weight, and 40 It is more preferable to use a material having a mass% to 55 mass% since the cohesive force in the shear direction and the peeling resistance can be improved.
なお、前記ゲル分率は、以下の式で算出することができる。
ゲル分率（質量％）＝｛（トルエンに浸漬した後の粘着剤層質量）／（トルエンに浸漬する前の粘着剤層質量）｝×１００
粘着剤層質量＝（導電性粘着シートの質量）−（基材の質量）−（導電性粒子の質量）The gel fraction can be calculated by the following formula.
Gel fraction (% by mass) = {(Adhesive layer mass after immersion in toluene) / (Adhesive layer mass before immersion in toluene)} × 100
Adhesive layer mass = (mass of conductive adhesive sheet)-(mass of substrate)-(mass of conductive particles)
前記架橋構造を備えた導電性粘着剤層を形成する場合、粘着剤としては、例えば前記アクリル系重合体等とともに、架橋剤を含有するものを使用することが好ましい。 When forming a conductive pressure-sensitive adhesive layer having the cross-linked structure, it is preferable to use, for example, a pressure-sensitive adhesive containing a cross-linking agent together with the acrylic polymer.
前記架橋剤としては、例えばイソシアネート系架橋剤、エポキシ系架橋剤、キレート系架橋剤、アジリジン系架橋剤等を使用することができる。前記架橋剤の種類は、前記アクリル系重合体が有する官能基に対応したものを使用することが好ましい。例えば前記アクリル系重合体としてカルボキシル基を有するものを使用する場合には、イソシアネート系架橋剤を使用することが好適である。 As said crosslinking agent, an isocyanate type crosslinking agent, an epoxy-type crosslinking agent, a chelate type crosslinking agent, an aziridine type crosslinking agent etc. can be used, for example. As the kind of the crosslinking agent, it is preferable to use one corresponding to the functional group of the acrylic polymer. For example, when using what has a carboxyl group as said acrylic polymer, it is suitable to use an isocyanate type crosslinking agent.
前記架橋剤は、前記導電性粘着剤層の前記ゲル分率が前記範囲となる量を選択し使用することが好ましい。 The cross-linking agent is preferably used by selecting an amount in which the gel fraction of the conductive pressure-sensitive adhesive layer falls within the above range.
前記導電性粘着剤層は、その粘着力をより一層向上することを目的として、粘着付与樹脂を含有していてもよい。 The conductive adhesive layer may contain a tackifying resin for the purpose of further improving the adhesive strength.
前記粘着付与樹脂としては、例えばロジン系樹脂、テルペン系樹脂、脂肪族（Ｃ５系）や芳香族（Ｃ９系）などの石油樹脂、スチレン系樹脂フェノール系樹脂、キシレン系樹脂、メタクリル系樹脂等を使用することができる。なかでも、前記粘着付与樹脂としては、ロジン系樹脂を使用することが好ましく、重合ロジン系樹脂を使用することがより好ましい。前記粘着付与樹脂の使用量は、（メタ）アクリル系重合体１００質量部に対し、１０質量部〜５０質量部の範囲であることが好ましい。 Examples of the tackifying resin include rosin resins, terpene resins, aliphatic (C5) and aromatic (C9) petroleum resins, styrene resins, phenol resins, xylene resins, methacrylic resins, and the like. Can be used. Among these, as the tackifying resin, it is preferable to use a rosin resin, and it is more preferable to use a polymerized rosin resin. It is preferable that the usage-amount of the said tackifying resin is the range of 10 mass parts-50 mass parts with respect to 100 mass parts of (meth) acrylic-type polymers.
前記導電性粘着剤層は、必要に応じて、各種添加剤を含有していてもよい。 The conductive adhesive layer may contain various additives as necessary.
上記添加剤としては、例えば可塑剤、軟化剤、金属不活性剤、酸化防止剤、顔料、染料等を使用することができる。 As said additive, a plasticizer, a softener, a metal deactivator, antioxidant, a pigment, dye etc. can be used, for example.
前記導電性粘着剤層の形成に使用可能な粘着剤としては、所定量の前記導電性物質と、前記粘着剤成分とを含有するものを使用することができる。 As the pressure-sensitive adhesive that can be used for forming the conductive pressure-sensitive adhesive layer, one containing a predetermined amount of the conductive substance and the pressure-sensitive adhesive component can be used.
また、前記導電性粘着剤層としては、トリアゾール系化合物を含有するものを使用することができる。 Moreover, what contains a triazole type compound can be used as the said electroconductive adhesive layer.
前記トリアゾール化合物としては、例えばベンゾトリアゾール、トリルトリアゾール及びそのカリウム塩、３−（Ｎ−サリチロイル）アミノ−１，２，４トリアゾール、２−（２’−ヒドロキシ５メチルフェニル）ベンゾトリアゾール等を使用することができ、ベンゾトリアゾールを使用することが、優れた接着保持力と、高温高湿度環境下に放置された場合に生じうる接着強さの低下を抑制できるため特に好ましい。 As the triazole compound, for example, benzotriazole, tolyltriazole and its potassium salt, 3- (N-salicyloyl) amino-1,2,4 triazole, 2- (2′-hydroxy-5methylphenyl) benzotriazole and the like are used. In particular, the use of benzotriazole is particularly preferable because it can suppress a decrease in adhesion strength that can be generated when left in an environment of high temperature and high humidity.
前記トリアゾール系化合物は、アクリル系粘着剤組成物１００質量部（固形分）に対し、０．０５質量部〜３．０質量部の範囲で使用することが好ましく、０．１質量部〜１．５質量部の範囲で使用することがより好ましく、０．３質量部〜１．０質量部の範囲で使用することが、優れた接着保持力と、高温高湿度環境下に放置された場合に生じうる接着強さの低下を抑制できるためさらに好ましい。 The triazole-based compound is preferably used in a range of 0.05 to 3.0 parts by mass with respect to 100 parts by mass (solid content) of the acrylic pressure-sensitive adhesive composition, and 0.1 to 1 part by mass. It is more preferable to use in the range of 5 parts by mass, and use in the range of 0.3 parts by mass to 1.0 part by mass has excellent adhesion retention and when left in a high temperature and high humidity environment. It is more preferable because it can suppress a decrease in adhesive strength that may occur.
前記方法で得られた粘着剤は、もっぱら導電性粘着剤層の形成に使用することができる。前記粘着剤の固形分は、１０質量％〜７０質量％の範囲であることが好ましく、３０質量％〜５５質量％の範囲であることがより好ましく、４３質量％〜５０質量％の範囲であることがさらに好ましい。 The pressure-sensitive adhesive obtained by the above method can be used exclusively for forming a conductive pressure-sensitive adhesive layer. The solid content of the pressure-sensitive adhesive is preferably in the range of 10% by mass to 70% by mass, more preferably in the range of 30% by mass to 55% by mass, and in the range of 43% by mass to 50% by mass. More preferably.
本発明の導電性粘着シートは、例えば剥離フィルムの表面に前記粘着剤を、ロールコーターやダイコーター等を用いて塗布し、その塗布層を５０℃〜１２０℃程度の環境下で乾燥し溶媒を除去することによって導電性粘着層を形成する工程、次に導電性粘着層を、前記導電性基材の両方の面に積層し、必要に応じて熱ラミネート等する工程、次に、必要に応じて１５℃〜５０℃程度の温度で４８時間〜１６８時間程度養生する工程を経ることによって製造することができる。 The conductive pressure-sensitive adhesive sheet of the present invention is prepared by, for example, applying the pressure-sensitive adhesive on the surface of a release film using a roll coater or a die coater, and drying the coating layer in an environment of about 50 ° C. to 120 ° C. A step of forming a conductive adhesive layer by removing, then a step of laminating the conductive adhesive layer on both surfaces of the conductive base material, and performing a heat lamination, etc., if necessary; Can be produced by passing through a step of curing at a temperature of about 15 ° C. to 50 ° C. for about 48 hours to 168 hours.
前記熱ラミネートは、４０℃〜１２０℃で行うことが好ましく、５０℃〜１００℃で行うことがより好ましく、６０℃〜９０℃で行うことがさらに好ましい。 The thermal lamination is preferably performed at 40 ° C to 120 ° C, more preferably 50 ° C to 100 ° C, and further preferably 60 ° C to 90 ° C.
また、本発明の導電性粘着シートとしては、それが被着体に貼付される前までフィルムが積層されたものであってもよい。 Moreover, as a conductive adhesive sheet of this invention, the film may be laminated | stacked until it is affixed on a to-be-adhered body.
前記剥離フィルムとしては、例えばクラフト紙、グラシン紙、上質紙等の紙；ポリエチレン、ポリプロピレン（ＯＰＰ、ＣＰＰ）、ポリエチレンテレフタレート等の樹脂フィルム；前記紙と樹脂フィルムとを積層したラミネート紙、前記紙にクレーやポリビニルアルコールなどで目止め処理を施したものの片面もしくは両面に、シリコーン系樹脂等の剥離処理を施したもの等を用いることができる。 Examples of the release film include paper such as kraft paper, glassine paper, and high-quality paper; resin films such as polyethylene, polypropylene (OPP, CPP), and polyethylene terephthalate; laminated paper obtained by laminating the paper and resin film; A material obtained by applying a release treatment such as a silicone-based resin to one or both surfaces of a material subjected to a sealing treatment with clay or polyvinyl alcohol can be used.
本発明の導電性粘着シートの好適な構成の例を図１及び図２に示す。図１は、導電性基材１上に導電性粘着剤層２を積層した片面粘着シートである。また、図２は、導電性基材１の両面に導電性粘着剤層２を積層した両面粘着シートである。これら構成においては、粘着剤層２の表面に、剥離フィルムが設けられた構成を好ましく使用できる。
The example of the suitable structure of the electroconductive adhesive sheet of this invention is shown in FIG.1 and FIG.2. FIG. 1 is a single-sided pressure-sensitive adhesive sheet in which a conductive pressure-
本発明の導電性粘着シートは、柔軟性に優れ、被着体への良好な接着性と導電性とリワーク性を有するため、電気、電子機器等に用いる電磁波のシールド用、静電気帯電防止の接地固定用として有用である。特に、凸凹部があり、導電性粘着シートの貼付けが難しい携帯電子機器等の小型電子端末の内蔵部品に貼り付けて使用する用途に好適に適用できる。 The conductive pressure-sensitive adhesive sheet of the present invention is excellent in flexibility and has good adhesion to the adherend, conductivity and reworkability. Therefore, the conductive pressure-sensitive adhesive sheet is used for shielding electromagnetic waves used in electrical and electronic equipment, and for antistatic grounding. Useful for fixation. In particular, it can be suitably applied to applications in which there are convex and concave portions and affixed to a built-in component of a small electronic terminal such as a portable electronic device in which it is difficult to apply a conductive adhesive sheet.
以下に実施例について具体的に説明する。 Examples will be specifically described below.
製造例１［導電性基材（Ａ）］
三木特種製紙株式会社製の湿式ポリエステル不織布「タイプＡ」（坪量１０ｇ／ｍ２、厚さ１５μｍ、ポリエステル繊維の直径５μｍ（平均径））を、塩化第一錫１０ｇ／ｌ、塩酸２０ｍｌ／ｌを含んだ水溶液に常温で約５分間浸漬し、その後、水洗いした。Production Example 1 [Conductive Substrate (A)]
Wet polyester nonwoven fabric “Type A” (basis weight 10 g / m 2 , thickness 15 μm, polyester fiber diameter 5 μm (average diameter)) manufactured by Miki Tokushu Paper Co., Ltd., stannous chloride 10 g / l, hydrochloric acid 20 ml / l Was immersed in an aqueous solution containing about 5 minutes at room temperature, and then washed with water.
次に、前記水洗いしたものを、塩化パラジウム１ｇ／ｌ及び塩酸２０ｍｌ／ｌを含む水溶液に常温で約１０分浸漬し、その後、水洗いした。 Next, the washed product was immersed in an aqueous solution containing 1 g / l of palladium chloride and 20 ml / l of hydrochloric acid at room temperature for about 10 minutes, and then washed with water.
次に、前記水洗いしたものを、硫酸銅１０ｇ／ｌ、ホルムアルデヒド７ｍｌ／ｌ、水酸化ナトリウム８ｇ／ｌ、エチレンジアミン４酢酸４ナトリウム（ＥＤＴＡ−４Ｎａ）３０ｇ／ｌ及び安定剤０．２５ｍｌ／ｌを含む４０℃に調整した無電解メッキ液に２０分浸漬し、その後、水洗いすることによって、無電解メッキ処理された湿式ポリエステル不織布を得た。 Next, the water-washed product contains 10 g / l copper sulfate, 7 ml / l formaldehyde, 8 g / l sodium hydroxide, 30 g / l ethylenediaminetetraacetic acid (EDTA-4Na) and 0.25 ml / l stabilizer. A wet polyester nonwoven fabric subjected to electroless plating was obtained by immersing in an electroless plating solution adjusted to 40 ° C. for 20 minutes and then washing with water.
次に、前記無電解メッキ処理された湿式ポリエステル不織布を、電解銅メッキ液（奥野製薬工業株式会社製、トップルチナＳＦ）に浸漬し、前記電解銅メッキ液による銅のメッキ量が６ｇ／ｍ２となるよう電解銅メッキ処理することによって、電解銅メッキ処理された湿式ポリエステル不織布を得た。Next, the electroless-plated wet polyester nonwoven fabric is immersed in an electrolytic copper plating solution (Okuno Pharmaceutical Co., Ltd., Top Lucina SF), and the copper plating amount by the electrolytic copper plating solution is 6 g / m 2 . By performing the electrolytic copper plating process, a wet polyester nonwoven fabric subjected to the electrolytic copper plating process was obtained.
次に、前記電解銅メッキ処理された湿式ポリエステル不織布を、硫酸ニッケル２４０ｇ／ｌ、塩化ニッケル４５ｇ／ｌ、ホウ酸３０ｇ／ｌ、サッカリン２ｇ／ｌ及び１，４−ブチンジオール０．２ｇ／ｌを含む電解ニッケルメッキ液に浸漬し、前記電解ニッケルメッキ液によるニッケルのメッキ量が４ｇ／ｍ２となるよう電解ニッケルメッキ処理し、水洗いし、乾燥させることによって、導電性基材（Ａ）を作製した。Next, the electrolytic copper-plated wet polyester non-woven fabric was mixed with nickel sulfate 240 g / l, nickel chloride 45 g / l, boric acid 30 g / l, saccharin 2 g / l and 1,4-butynediol 0.2 g / l. A conductive base material (A) is produced by immersing in an electrolytic nickel plating solution, electrolytic nickel plating so that the nickel plating amount by the electrolytic nickel plating solution is 4 g / m 2 , washing with water and drying. did.
製造例２［導電性基材（Ｂ）］
三木特種製紙株式会社製の湿式ポリエステル不織布「タイプＡ」の代わりに、旭化成株式会社製の湿式ポリエステル不織布「シルキーファインＷＳ７Ａ−０５−６」（坪量６ｇ／ｍ２、厚さ１８μｍ、ポリエステル繊維の直径４．５μｍ（平均径））を使用したこと以外は、製造例１と同様の方法で導電性基材（Ｂ）を作製した。Production Example 2 [Conductive Substrate (B)]
Instead of wet polyester nonwoven fabric “Type A” manufactured by Miki Tokushu Paper Co., Ltd., wet polyester nonwoven fabric “Silky Fine WS7A-05-6” manufactured by Asahi Kasei Co., Ltd. (basis weight 6 g / m 2 , thickness 18 μm, polyester fiber A conductive substrate (B) was produced in the same manner as in Production Example 1 except that a diameter of 4.5 μm (average diameter) was used.
製造例３［導電性基材（Ｃ）］
三木特種製紙株式会社製の湿式ポリエステル不織布「タイプＡ」の代わりに、旭化成株式会社製の湿式ポリエステル不織布「シルキーファインＷＳ７Ａ−０４」（坪量４ｇ／ｍ２、厚さ１６μｍ、ポリエステル繊維の直径４．５μｍ（平均径））を使用したこと以外は、製造例１と同様の方法で導電性基材（Ｃ）を作製した。Production Example 3 [Conductive Substrate (C)]
Instead of wet polyester nonwoven fabric “Type A” manufactured by Miki Tokushu Paper Co., Ltd., wet polyester nonwoven fabric “Silky Fine WS7A-04” manufactured by Asahi Kasei Corporation (basis weight 4 g / m 2 , thickness 16 μm, polyester fiber diameter 4 A conductive substrate (C) was produced in the same manner as in Production Example 1 except that .5 μm (average diameter) was used.
製造例４［導電性基材（Ｄ）］
三木特種製紙株式会社製の湿式ポリエステル不織布「タイプＡ」の代わりに、日本製紙パピリア株式会社製の湿式ポリエステル不織布「５．５ｇ／ｍ２」（坪量５．５ｇ／ｍ２、厚さ１４μｍ、ポリエステル繊維の直径４．５μｍ（平均径））を使用したこと以外は、製造例１と同様の方法で導電性基材（Ｄ）を作製した。Production Example 4 [Conductive Substrate (D)]
Instead of wet polyester nonwoven fabric “Type A” manufactured by Miki Tokushu Paper Co., Ltd., wet polyester nonwoven fabric “5.5 g / m 2 ” (basis weight: 5.5 g / m 2 , thickness: 14 μm, manufactured by Nippon Paper Papillia Co., Ltd. A conductive substrate (D) was produced in the same manner as in Production Example 1 except that polyester fiber diameter 4.5 μm (average diameter) was used.
製造例５［導電性基材（Ｅ）］
常温下、三木特種製紙株式会社製の湿式ポリエステル不織布「タイプＡ」（坪量１０ｇ／ｍ２、厚さ１５μｍ、ポリエステル繊維の直径５μｍ（平均径））を、塩化第一錫１０ｇ／ｌ及び塩酸２０ｍｌ／ｌを含有する水溶液に約５分間浸漬し、水洗いした後、塩化パラジウム１ｇ／ｌ及び塩酸２０ｍｌ／ｌを含む水溶液に約１０分浸漬し、水洗いした。Production Example 5 [conductive substrate (E)]
Wet polyester nonwoven fabric “Type A” (basis weight 10 g / m 2 , thickness 15 μm, polyester fiber diameter 5 μm (average diameter)) manufactured by Miki Tokushu Paper Co., Ltd. at room temperature, stannous chloride 10 g / l and hydrochloric acid After immersing in an aqueous solution containing 20 ml / l for about 5 minutes and washing with water, it was immersed in an aqueous solution containing 1 g / l of palladium chloride and 20 ml / l of hydrochloric acid for about 10 minutes and washed with water.
次に、前記水洗いしたものを、硫酸銅１０ｇ／ｌ、ホルムアルデヒド７ｍｌ／ｌ、水酸化ナトリウム８ｇ／ｌ、エチレンジアミン４酢酸４ナトリウム（ＥＤＴＡ−４Ｎａ）３０ｇ／ｌ及び安定剤（０．２５ｍｌ／ｌ）を含む４０℃に調整した無電解メッキ液に、６０分浸漬し、前記無電解メッキ液による銅のメッキ量が６ｇ／ｍ２となるよう無電解メッキ処理した後、水洗し、乾燥させることによって、導電性基材（Ｅ）を作製した。Next, what was washed with water was 10 g / l copper sulfate, 7 ml / l formaldehyde, 8 g / l sodium hydroxide, 30 g / l ethylenediaminetetraacetic acid (EDTA-4Na), and a stabilizer (0.25 ml / l). After being immersed in an electroless plating solution adjusted to 40 ° C. containing 60 minutes and subjected to electroless plating so that the amount of copper plating by the electroless plating solution is 6 g / m 2 , washing with water and drying are performed. A conductive substrate (E) was prepared.
製造例６［導電性基材（Ｆ）］
常温下、三木特種製紙株式会社製の湿式ポリエステル不織布「タイプＡ」（坪量１０ｇ／ｍ２、厚さ１５μｍ、ポリエステル繊維の直径５μｍ（平均径））を、塩化第一錫１０ｇ／ｌ及び塩酸２０ｍｌ／ｌを含む水溶液に約５分間浸漬し、水洗いした後、塩化パラジウム１ｇ／ｌ及び塩酸２０ｍｌ／ｌを含む水溶液に約１０分浸漬し、水洗いした。Production Example 6 [Conductive Substrate (F)]
Wet polyester nonwoven fabric “Type A” (basis weight 10 g / m 2 , thickness 15 μm, polyester fiber diameter 5 μm (average diameter)) manufactured by Miki Tokushu Paper Co., Ltd. at room temperature, stannous chloride 10 g / l and hydrochloric acid After immersing in an aqueous solution containing 20 ml / l for about 5 minutes and washing with water, it was immersed in an aqueous solution containing 1 g / l of palladium chloride and 20 ml / l of hydrochloric acid for about 10 minutes and washed with water.
次に、前記水洗いしたものを、硫酸ニッケル２０ｇ／ｌ、クエン酸ナトリウム３０ｇ／ｌ、次亜リン酸ナトリウム１５ｇ／ｌ及び塩化アンモニウム３０ｇ／ｌを含有し、アンモニア水でｐＨ９．５に調整された４０℃の無電解メッキ液に６０分浸漬し、前記無電解メッキ液によるニッケルのメッキ量が６ｇ／ｍ２となるよう無電解メッキ処理した後、水洗し、乾燥させることによって、導電性基材（Ｆ）を作製した。Next, the water-washed product contains nickel sulfate 20 g / l, sodium citrate 30 g / l, sodium hypophosphite 15 g / l and ammonium chloride 30 g / l, and adjusted to pH 9.5 with aqueous ammonia. The substrate is immersed in an electroless plating solution at 40 ° C. for 60 minutes, subjected to electroless plating so that the amount of nickel plated by the electroless plating solution is 6 g / m 2 , washed with water, and dried to form a conductive substrate. (F) was produced.
製造例７［導電性基材（Ｇ）］
常温下、三木特種製紙株式会社製の湿式ポリエステル不織布「タイプＡ」（坪量１０ｇ／ｍ２、厚さ１５μｍ、ポリエステル繊維の直径５μｍ（平均径））を、塩化第一錫１０ｇ／ｌ及び塩酸２０ｍｌ／ｌを含む水溶液に約５分間浸漬し、水洗いした後、塩化パラジウム１ｇ／ｌ及び塩酸２０ｍｌ／ｌを含む水溶液に約１０分浸漬し、水洗いした。Production Example 7 [Conductive substrate (G)]
Wet polyester nonwoven fabric “Type A” (basis weight 10 g / m 2 , thickness 15 μm, polyester fiber diameter 5 μm (average diameter)) manufactured by Miki Tokushu Paper Co., Ltd. at room temperature, stannous chloride 10 g / l and hydrochloric acid After immersing in an aqueous solution containing 20 ml / l for about 5 minutes and washing with water, it was immersed in an aqueous solution containing 1 g / l of palladium chloride and 20 ml / l of hydrochloric acid for about 10 minutes and washed with water.
次に、前記水洗いしたものを、硫酸銅１０ｇ／ｌ、ホルムアルデヒド７ｍｌ／ｌ、水酸化ナトリウム８ｇ／ｌ、エチレンジアミン４酢酸４ナトリウム（ＥＤＴＡ−４Ｎａ）３０ｇ／ｌ及び安定剤（０．２５ｍｌ／ｌ）を含む４０℃に調整された無電解銅メッキ液に６０分浸漬し、前記無電解銅メッキ液による銅のメッキ量を６ｇ／ｍ２となるよう無電解銅メッキ処理した後、水洗いすることによって、無電解銅メッキ処理された湿式ポリエステル不織布を得た。Next, what was washed with water was 10 g / l copper sulfate, 7 ml / l formaldehyde, 8 g / l sodium hydroxide, 30 g / l ethylenediaminetetraacetic acid (EDTA-4Na), and a stabilizer (0.25 ml / l). By immersing in an electroless copper plating solution adjusted to 40 ° C. containing 60 minutes, subjecting the electroless copper plating solution to a copper plating amount of 6 g / m 2, and then washing with water. A wet polyester nonwoven fabric subjected to electroless copper plating treatment was obtained.
次に、前記無電解銅メッキ処理された湿式ポリエステル不織布を、硫酸ニッケル２０ｇ／ｌ、クエン酸ナトリウム３０ｇ／ｌ、次亜リン酸ナトリウム１５ｇ／ｌ及び塩化アンモニウム３０ｇ／ｌを含有し、アンモニア水でｐＨ９．５に調整された４０℃の無電解ニッケルメッキ液に３０分浸漬し、前記無電解ニッケルメッキ液によるニッケルのメッキ量が４ｇ／ｍ２となるよう無電解ニッケルメッキ処理した後、水洗いすることによって、導電性基材（Ｇ）を作製した。Next, the electroless copper-plated wet polyester nonwoven fabric contains nickel sulfate 20 g / l, sodium citrate 30 g / l, sodium hypophosphite 15 g / l and ammonium chloride 30 g / l. It is immersed in an electroless nickel plating solution adjusted to pH 9.5 at 40 ° C. for 30 minutes, subjected to electroless nickel plating so that the amount of nickel plating by the electroless nickel plating solution is 4 g / m 2, and then washed with water. Thus, a conductive substrate (G) was produced.
製造例８［導電性基材（Ｈ）］
三木特種製紙株式会社製の湿式ポリエステル不織布「タイプＡ」（坪量１０ｇ／ｍ２、厚さ１５μｍ、ポリエステル繊維の直径５μｍ（平均径））を、塩化第一錫１０ｇ／ｌ、塩酸２０ｍｌ／ｌを含んだ水溶液に常温で約５分間浸漬し、その後、水洗いした。Production Example 8 [conductive substrate (H)]
Wet polyester nonwoven fabric “Type A” (basis weight 10 g / m 2 , thickness 15 μm, polyester fiber diameter 5 μm (average diameter)) manufactured by Miki Tokushu Paper Co., Ltd., stannous chloride 10 g / l, hydrochloric acid 20 ml / l Was immersed in an aqueous solution containing about 5 minutes at room temperature, and then washed with water.
次に、前記水洗いしたものを、塩化パラジウム１ｇ／ｌ及び塩酸２０ｍｌ／ｌを含む水溶液に常温で約１０分浸漬し、その後、水洗いした。 Next, the washed product was immersed in an aqueous solution containing 1 g / l of palladium chloride and 20 ml / l of hydrochloric acid at room temperature for about 10 minutes, and then washed with water.
次に、前記水洗いしたものを、硫酸銅１０ｇ／ｌ、ホルムアルデヒド７ｍｌ／ｌ、水酸化ナトリウム８ｇ／ｌ、エチレンジアミン４酢酸４ナトリウム（ＥＤＴＡ−４Ｎａ）３０ｇ／ｌ及び安定剤０．２５ｍｌ／ｌを含む４０℃に調整した無電解メッキ液に２０分浸漬し、その後、水洗いすることによって、無電解メッキ処理された湿式ポリエステル不織布を得た。 Next, the water-washed product contains 10 g / l copper sulfate, 7 ml / l formaldehyde, 8 g / l sodium hydroxide, 30 g / l ethylenediaminetetraacetic acid (EDTA-4Na) and 0.25 ml / l stabilizer. A wet polyester nonwoven fabric subjected to electroless plating was obtained by immersing in an electroless plating solution adjusted to 40 ° C. for 20 minutes and then washing with water.
次に、前記無電解メッキ処理された湿式ポリエステル不織布を、硫酸ニッケル２４０ｇ／ｌ、塩化ニッケル４５ｇ／ｌ、ホウ酸３０ｇ／ｌ、サッカリン２ｇ／ｌ及び１，４−ブチンジオール０．２ｇ／ｌを含む電解ニッケルメッキ液に浸漬し、前記電解ニッケルメッキ液によるニッケルのメッキ量が４ｇ／ｍ２となるよう電解ニッケルメッキ処理し、水洗いし、乾燥させることによって、導電性基材（Ｈ）を作製した。Next, the electroless-plated wet polyester non-woven fabric was charged with nickel sulfate 240 g / l, nickel chloride 45 g / l, boric acid 30 g / l, saccharin 2 g / l and 1,4-butynediol 0.2 g / l. A conductive base material (H) is produced by immersing in an electrolytic nickel plating solution, and subjecting the electrolytic nickel plating solution to electrolytic nickel plating so that the amount of nickel plating is 4 g / m 2 , washing with water, and drying. did.
製造例９［導電性基材（Ｉ）］
旭化成せんい株式会社製プレシゼ（乾式ポリエステル不織布に銅とニッケルがメッキ処理されたもの）を導電性基材（Ｉ）とした。Production Example 9 [Conductive Substrate (I)]
Asahi Kasei Fiber Co., Ltd. Presise (dry polyester nonwoven fabric plated with copper and nickel) was used as the conductive substrate (I).
製造例１０［導電性基材（Ｊ）］
三木特種製紙株式会社製の湿式ポリエステル不織布「タイプＡ」の代わりに、ＪＸ日鉱日石エネルギー株式会社製の乾式ポリエステル不織布「ミライフＴＹ０５０３ＦＥ」（坪量８ｇ／ｍ２、厚さ２８μｍ、ポリエステル繊維の直径１２μｍ（平均径））を用いたこと以外は、製造例１と同様の方法で導電性基材（Ｊ）を作製した。Production Example 10 [Conductive Substrate (J)]
Instead of wet polyester nonwoven fabric “Type A” manufactured by Miki Tokushu Paper Co., Ltd., dry polyester nonwoven fabric “Milife TY0503FE” manufactured by JX Nippon Mining & Energy Co., Ltd. (basis weight 8 g / m 2 , thickness 28 μm, polyester fiber diameter) A conductive substrate (J) was produced in the same manner as in Production Example 1 except that 12 μm (average diameter) was used.
製造例１１［導電性基材（Ｋ）］
［メッキ不織布Ｋ］
三木特種製紙株式会社製の湿式ポリエステル不織布「タイプＡ」の代わりに、ＪＸ日鉱日石エネルギー株式会社製の乾式ポリエステル不織布「ミライフＴ１０」（坪量１０ｇ／ｍ２、厚さ２８μｍ、ポリエステル繊維の直径１０μｍ（平均径））を用いたこと以外は、製造例１と同様の方法で導電性基材（Ｋ）を作製した。Production Example 11 [Conductive substrate (K)]
[Plating nonwoven fabric K]
Instead of wet polyester nonwoven fabric “Type A” manufactured by Miki Tokushu Paper Co., Ltd., dry polyester nonwoven fabric “Milife T10” manufactured by JX Nippon Mining & Energy Corporation (basis weight 10 g / m 2 , thickness 28 μm, polyester fiber diameter) A conductive substrate (K) was produced in the same manner as in Production Example 1 except that 10 μm (average diameter) was used.
製造例１２［導電性基材（Ｌ）］
三木特種製紙株式会社製の湿式ポリエステル不織布「タイプＡ」の代わりに、日本製紙パピリア株式会社製の湿式麻不織布「Ｄ５４Ｅ」（坪量１６ｇ／ｍ２、厚さ４３μｍ）を用いたこと以外は、製造例１と同様の方法で導電性基材（Ｌ）を作製した。Production Example 12 [Conductive Substrate (L)]
Except for using the wet polyester nonwoven fabric “D54E” (basis weight 16 g / m 2 , thickness 43 μm) manufactured by Nippon Paper Industries Papiria Co., Ltd. instead of the wet polyester nonwoven fabric “Type A” manufactured by Miki Tokushu Paper Co., Ltd. A conductive substrate (L) was produced in the same manner as in Production Example 1.
調製例１［アクリル系粘着剤組成物（１）の調製］
冷却管、撹拌機、温度計、滴下漏斗を備えた反応容器にｎ−ブチルアクリレート９６．４質量部、２−ヒドロキシエチルアクリレート０．１質量部、アクリル酸３．５質量部と重合開始剤として２，２’−アゾビスイソブチルニトリル０．１質量部を酢酸エチル１００質量部に溶解し、反応容器内を窒素置換した後、８０℃で１２時間重合させることによって、重量平均分子量６０万のアクリル系共重合体溶液を得た。Preparation Example 1 [Preparation of acrylic pressure-sensitive adhesive composition (1)]
In a reaction vessel equipped with a condenser, a stirrer, a thermometer, and a dropping funnel, 96.4 parts by mass of n-butyl acrylate, 0.1 part by mass of 2-hydroxyethyl acrylate, 3.5 parts by mass of acrylic acid and a polymerization initiator After dissolving 0.1 parts by mass of 2,2′-azobisisobutylnitrile in 100 parts by mass of ethyl acetate and purging the inside of the reaction vessel with nitrogen, polymerization is carried out at 80 ° C. for 12 hours, whereby an acrylic having a weight average molecular weight of 600,000 is obtained. A system copolymer solution was obtained.
前記アクリル系共重合体溶液の固形分１００質量部に対し、重合ロジンペンタエリスリトールエステル（荒川化学工業（株）製、ペンセルＤ−１３５、軟化点１３５℃）１０質量部、不均化ロジングリセリンエステル（荒川化学工業（株）製、スーパーエステルＡ−１００、軟化点１００℃）１０質量部を配合し、酢酸エチルを用いて、前記アクリル系共重合体の固形分濃度を４５質量％に調整することによってアクリル系粘着剤組成物（１）を得た。 10 parts by mass of polymerized rosin pentaerythritol ester (Arakawa Chemical Industries, Pencel D-135, softening point 135 ° C.), disproportionated rosin glycerin ester with respect to 100 parts by mass of the solid content of the acrylic copolymer solution. (Arakawa Chemical Industries, Ltd., Superester A-100, softening point 100 ° C.) is mixed with 10 parts by mass, and the solid content concentration of the acrylic copolymer is adjusted to 45% by mass using ethyl acetate. As a result, an acrylic pressure-sensitive adhesive composition (1) was obtained.
調製例２［アクリル系粘着剤組成物（２）の調製］
冷却管、撹拌機、温度計、滴下漏斗を備えた反応容器にｎ−ブチルアクリレート９９．９質量部、２−ヒドロキシエチルアクリレート０．１質量部、重合開始剤として２，２’−アゾビスイソブチルニトリル０．１質量部を酢酸エチル１００質量部に溶解し、反応容器内を窒素置換した後、８０℃で１２時間重合させることによって、重量平均分子量６０万のアクリル系共重合体溶液を得た。Preparation Example 2 [Preparation of acrylic pressure-sensitive adhesive composition (2)]
In a reaction vessel equipped with a condenser, a stirrer, a thermometer, and a dropping funnel, 99.9 parts by mass of n-butyl acrylate, 0.1 part by mass of 2-hydroxyethyl acrylate, 2,2′-azobisisobutyl as a polymerization initiator 0.1 parts by mass of nitrile was dissolved in 100 parts by mass of ethyl acetate, the inside of the reaction vessel was purged with nitrogen, and then polymerized at 80 ° C. for 12 hours to obtain an acrylic copolymer solution having a weight average molecular weight of 600,000. .
前記アクリル系共重合体溶液の固形分１００質量部に対し、重合ロジンペンタエリスリトールエステル（荒川化学工業（株）製、ペンセルＤ−１３５、軟化点１３５℃）１０質量部、不均化ロジングリセリンエステル（荒川化学工業（株）製、スーパーエステルＡ−１００、軟化点１００℃）１０質量部を配合し、酢酸エチルを用いて、前記アクリル系共重合体の固形分濃度を４５質量％に調整することによってアクリル系粘着剤組成物（２）を得た。 10 parts by mass of polymerized rosin pentaerythritol ester (Arakawa Chemical Industries, Pencel D-135, softening point 135 ° C.), disproportionated rosin glycerin ester with respect to 100 parts by mass of the solid content of the acrylic copolymer solution. (Arakawa Chemical Industries, Ltd., Superester A-100, softening point 100 ° C.) is mixed with 10 parts by mass, and the solid content concentration of the acrylic copolymer is adjusted to 45% by mass using ethyl acetate. As a result, an acrylic pressure-sensitive adhesive composition (2) was obtained.
調製例３［アクリル系粘着剤組成物（３）の調製］
冷却管、撹拌機、温度計、滴下漏斗を備えた反応容器にｎ−ブチルアクリレート９２．９質量部、２−ヒドロキシエチルアクリレート０．１質量部、アクリル酸７質量部、重合開始剤として２，２’−アゾビスイソブチルニトリル０．１質量部を酢酸エチル１００質量部に溶解し、反応容器内を窒素置換した後、８０℃で１２時間重合させることによって、重量平均分子量６０万のアクリル系共重合体溶液を得た。Preparation Example 3 [Preparation of acrylic pressure-sensitive adhesive composition (3)]
In a reaction vessel equipped with a condenser, a stirrer, a thermometer, and a dropping funnel, 92.9 parts by mass of n-butyl acrylate, 0.1 part by mass of 2-hydroxyethyl acrylate, 7 parts by mass of acrylic acid, 2 as a polymerization initiator An acrylic copolymer having a weight average molecular weight of 600,000 is obtained by dissolving 0.1 part by weight of 2′-azobisisobutylnitrile in 100 parts by weight of ethyl acetate, purging the inside of the reaction vessel with nitrogen, and polymerizing at 80 ° C. for 12 hours. A polymer solution was obtained.
前記アクリル系共重合体溶液の固形分１００質量部に対し、重合ロジンペンタエリスリトールエステル（荒川化学工業（株）製、ペンセルＤ−１３５、軟化点１３５℃）１０質量部、不均化ロジングリセリンエステル（荒川化学工業（株）製、スーパーエステルＡ−１００、軟化点１００℃）１０質量部を配合し、酢酸エチルを用いて、前記アクリル系共重合体の固形分濃度を４５質量％に調整することによってアクリル系粘着剤組成物（３）を得た。 10 parts by mass of polymerized rosin pentaerythritol ester (Arakawa Chemical Industries, Pencel D-135, softening point 135 ° C.), disproportionated rosin glycerin ester with respect to 100 parts by mass of the solid content of the acrylic copolymer solution. (Arakawa Chemical Industries, Ltd., Superester A-100, softening point 100 ° C.) is mixed with 10 parts by mass, and the solid content concentration of the acrylic copolymer is adjusted to 45% by mass using ethyl acetate. As a result, an acrylic pressure-sensitive adhesive composition (3) was obtained.
調製例４［アクリル系粘着剤組成物（４）の調製］
冷却管、撹拌機、温度計、滴下漏斗を備えた反応容器にｎ−ブチルアクリレート９７．４質量部、２−ヒドロキシエチルアクリレート０．１質量部、アクリル酸２．５質量部、重合開始剤として２，２’−アゾビスイソブチルニトリル０．１質量部を酢酸エチル１００質量部に溶解し、反応容器内を窒素置換した後、８０℃で１２時間重合させることによって、重量平均分子量６０万のアクリル系共重合体溶液を得た。Preparation Example 4 [Preparation of acrylic pressure-sensitive adhesive composition (4)]
In a reaction vessel equipped with a condenser, a stirrer, a thermometer, and a dropping funnel, 97.4 parts by mass of n-butyl acrylate, 0.1 part by mass of 2-hydroxyethyl acrylate, 2.5 parts by mass of acrylic acid, as a polymerization initiator After dissolving 0.1 parts by mass of 2,2′-azobisisobutylnitrile in 100 parts by mass of ethyl acetate and purging the inside of the reaction vessel with nitrogen, polymerization is carried out at 80 ° C. for 12 hours, whereby an acrylic having a weight average molecular weight of 600,000 is obtained. A system copolymer solution was obtained.
前記アクリル系共重合体溶液の固形分１００質量部に対し、重合ロジンペンタエリスリトールエステル（荒川化学工業（株）製、ペンセルＤ−１３５、軟化点１３５℃）１０質量部、不均化ロジングリセリンエステル（荒川化学工業（株）製、スーパーエステルＡ−１００、軟化点１００℃）１０質量部を配合し、酢酸エチルを用いて、前記アクリル系共重合体の固形分濃度を４５質量％に調整することによってアクリル系粘着剤組成物（４）を得た。 10 parts by mass of polymerized rosin pentaerythritol ester (Arakawa Chemical Industries, Pencel D-135, softening point 135 ° C.), disproportionated rosin glycerin ester with respect to 100 parts by mass of the solid content of the acrylic copolymer solution. (Arakawa Chemical Industries, Ltd., Superester A-100, softening point 100 ° C.) is mixed with 10 parts by mass, and the solid content concentration of the acrylic copolymer is adjusted to 45% by mass using ethyl acetate. As a result, an acrylic pressure-sensitive adhesive composition (4) was obtained.
調製例５［導電性粘着剤組成物（１Ａ−１）の調製］
前記アクリル系粘着剤組成物（１）１００質量部（固形分４５質量％）と、福田金属箔粉工業株式会社製のニッケル粉「ＮＩ１２３Ｊ」（粒子径ｄ５０：６．３μｍ、粒子径ｄ８５：１０．０μｍ、タップ密度：４．３ｇ／ｃｍ３、インコリミテッド社「ＮＩ１２３」を平滑化処理したもの）２２．５質量部と、架橋剤としてバーノックＮＣ４０（ＤＩＣ株式会社製のイソシアネート系架橋剤、固形分４０質量％）２．５質量部と、ベンゾトリアゾール０．２３質量部とを混合し、酢酸エチルを用い固形分濃度を４７質量％に調整したものを、分散攪拌機を用いて１０分間撹拌することによって導電性粘着剤（１Ａ−１）を得た。Preparation Example 5 [Preparation of conductive adhesive composition (1A-1)]
100 parts by weight of the acrylic pressure-sensitive adhesive composition (1) (solid content: 45% by weight) and nickel powder “NI123J” manufactured by Fukuda Metal Foil Powder Co., Ltd. (particle diameter d50: 6.3 μm, particle diameter d85: 10) 0.0 μm, tap density: 4.3 g / cm 3 , 22.5 parts by mass of Inco Ltd. “NI123”) and Vernock NC40 (an isocyanate-based crosslinking agent manufactured by DIC Corporation, solid) as a crosslinking agent (Min. 40% by mass) 2.5 parts by mass and 0.23 parts by mass of benzotriazole were mixed, and the solid content concentration adjusted to 47% by mass using ethyl acetate was stirred for 10 minutes using a dispersion stirrer. As a result, a conductive pressure-sensitive adhesive (1A-1) was obtained.
調製例６［導電性粘着剤組成物（１Ａ−２）の調製］
福田金属箔粉工業株式会社製のニッケル粉「ＮＩ１２３Ｊ」の使用量を２２．５質量部から９質量部に変更したこと以外は、調製例５と同様の方法で導電性粘着剤（１Ａ−２）を得た。Preparation Example 6 [Preparation of conductive adhesive composition (1A-2)]
A conductive adhesive (1A-2) was prepared in the same manner as in Preparation Example 5 except that the amount of nickel powder “NI123J” manufactured by Fukuda Metal Foil Powder Co., Ltd. was changed from 22.5 parts by mass to 9 parts by mass. )
調製例７［導電性粘着剤組成物（１Ａ−３）の調製］
福田金属箔粉工業株式会社製のニッケル粉「ＮＩ１２３Ｊ」の使用量を２２．５質量部から３６質量部に変更したこと以外は、調製例５と同様の方法で導電性粘着剤（１Ａ−３）を得た。Preparation Example 7 [Preparation of conductive adhesive composition (1A-3)]
A conductive adhesive (1A-3) was prepared in the same manner as in Preparation Example 5, except that the amount of nickel powder “NI123J” manufactured by Fukuda Metal Foil Powder Co., Ltd. was changed from 22.5 parts by mass to 36 parts by mass. )
調製例８［導電性粘着剤組成物（１Ａ−４）の調製］
福田金属箔粉工業株式会社製のニッケル粉「ＮＩ１２３Ｊ」の使用量を２２．５質量部から０質量部に変更したこと以外は、調製例５と同様の方法で導電性粘着剤（１Ａ−４）を得た。Preparation Example 8 [Preparation of conductive adhesive composition (1A-4)]
A conductive adhesive (1A-4) was prepared in the same manner as in Preparation Example 5, except that the amount of nickel powder “NI123J” manufactured by Fukuda Metal Foil Powder Co., Ltd. was changed from 22.5 parts by mass to 0 parts by mass. )
調製例９［導電性粘着剤組成物（１Ａ−５）の調製］
福田金属箔粉工業株式会社製のニッケル粉「ＮＩ１２３Ｊ」の使用量を２２．５質量部から６７．５質量部に変更したこと以外は、調製例５と同様の方法で導電性粘着剤（１Ａ−５）を得た。Preparation Example 9 [Preparation of conductive adhesive composition (1A-5)]
The conductive adhesive (1A) was prepared in the same manner as in Preparation Example 5, except that the amount of nickel powder “NI123J” manufactured by Fukuda Metal Foil Powder Co., Ltd. was changed from 22.5 parts by mass to 67.5 parts by mass. -5) was obtained.
調製例１０［導電性粘着剤組成物（２Ａ）の調製］
前記アクリル系粘着剤組成物（１）の代わりに、前記アクリル系粘着剤組成物（２）を使用すること以外は、調製例５と同様の方法で導電性粘着剤（２Ａ）を得た。Preparation Example 10 [Preparation of conductive adhesive composition (2A)]
A conductive pressure-sensitive adhesive (2A) was obtained in the same manner as in Preparation Example 5, except that the acrylic pressure-sensitive adhesive composition (2) was used instead of the acrylic pressure-sensitive adhesive composition (1).
調製例１１［導電性粘着剤組成物（３Ａ）の調製］
前記アクリル系粘着剤組成物（１）の代わりに、前記アクリル系粘着剤組成物（３）を使用すること以外は、調製例５と同様の方法で導電性粘着剤（３Ａ）を得た。Preparation Example 11 [Preparation of conductive adhesive composition (3A)]
A conductive pressure-sensitive adhesive (3A) was obtained in the same manner as in Preparation Example 5, except that the acrylic pressure-sensitive adhesive composition (3) was used instead of the acrylic pressure-sensitive adhesive composition (1).
調製例１２［導電性粘着剤組成物（４Ａ）の調製］
前記アクリル系粘着剤組成物（１）の代わりに、前記アクリル系粘着剤組成物（４）を使用すること以外は、調製例５と同様の方法で導電性粘着剤（４Ａ）を得た。Preparation Example 12 [Preparation of conductive adhesive composition (4A)]
A conductive adhesive (4A) was obtained in the same manner as in Preparation Example 5, except that the acrylic adhesive composition (4) was used instead of the acrylic adhesive composition (1).
調製例１３［導電性粘着剤組成物（１Ｂ）の調製］
福田金属箔粉工業株式会社製のニッケル粉「ＮＩ１２３Ｊ」の代わりに、インコリミテッド社製のニッケル粉「ＮＩ１２３」（粒子径ｄ５０：１０．７、粒子径ｄ８５：２５．０μｍ）を２２．５質量部使用したこと以外は、調製例５と同様の方法で導電性粘着剤（１Ｂ）を得た。Preparation Example 13 [Preparation of conductive adhesive composition (1B)]
Instead of the nickel powder “NI123J” manufactured by Fukuda Metal Foil Powder Co., Ltd., 22.5 mass of nickel powder “NI123” (particle diameter d50: 10.7, particle diameter d85: 25.0 μm) manufactured by Incori Ltd. A conductive pressure-sensitive adhesive (1B) was obtained in the same manner as in Preparation Example 5, except that a part of the product was used.
（実施例１）
前記導電性粘着剤組成物（１Ａ−１）を、ニッパ株式会社製の剥離フィルム「ＰＥＴ３８×１ Ａ３」上に、乾燥後の導電性粘着剤層の厚さが９μｍになるようにコンマコーターを用いて塗工し、８０℃に設定した乾燥器で２分間乾燥させることによって導電性粘着剤層を作製した。Example 1
Apply a comma coater to the conductive adhesive composition (1A-1) on a release film “PET38 × 1 A3” manufactured by Nipper Corporation so that the thickness of the conductive adhesive layer after drying is 9 μm. The conductive pressure-sensitive adhesive layer was prepared by applying and drying for 2 minutes in a drier set at 80 ° C.
次に、前記導電性粘着剤層を、前記導電性基材（Ａ）の両面に貼付し、それらを８０℃で熱ラミネートし、次いで４０℃で４８時間養生することによって導電性粘着シートを作製した。 Next, the conductive pressure-sensitive adhesive layer is pasted on both sides of the conductive base material (A), they are thermally laminated at 80 ° C., and then cured at 40 ° C. for 48 hours to produce a conductive pressure-sensitive adhesive sheet. did.
（実施例２）
導電性基材（Ａ）の代わりに、導電性基材（Ｂ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 2)
A conductive adhesive sheet was produced in the same manner as in Example 1 except that the conductive substrate (B) was used instead of the conductive substrate (A).
（実施例３）
導電性基材（Ａ）の代わりに、導電性基材（Ｃ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 3)
A conductive adhesive sheet was produced in the same manner as in Example 1 except that the conductive substrate (C) was used instead of the conductive substrate (A).
（実施例４）
導電性基材（Ａ）の代わりに、導電性基材（Ｄ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。Example 4
A conductive adhesive sheet was produced in the same manner as in Example 1 except that the conductive substrate (D) was used instead of the conductive substrate (A).
（実施例５）
導電性粘着剤組成物（１Ａ−１）の代わりに、導電性粘着剤組成物（１Ａ−２）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 5)
A conductive pressure-sensitive adhesive sheet was produced in the same manner as in Example 1 except that the conductive pressure-sensitive adhesive composition (1A-2) was used instead of the conductive pressure-sensitive adhesive composition (1A-1).
（実施例６）
導電性粘着剤組成物（１Ａ−１）の代わりに、導電性粘着剤組成物（１Ａ−３）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 6)
A conductive pressure-sensitive adhesive sheet was produced in the same manner as in Example 1 except that the conductive pressure-sensitive adhesive composition (1A-3) was used instead of the conductive pressure-sensitive adhesive composition (1A-1).
（実施例７）
導電性粘着剤組成物（１Ａ−１）の代わりに、導電性粘着剤組成物（２Ａ）を使用し、かつ、養生時間を４８時間から１２０時間に変更したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 7)
The same as Example 1 except that instead of the conductive adhesive composition (1A-1), the conductive adhesive composition (2A) was used and the curing time was changed from 48 hours to 120 hours. A conductive pressure-sensitive adhesive sheet was prepared by the method described above.
（実施例８）
導電性粘着剤組成物（１Ａ−１）の代わりに、導電性粘着剤組成物（３Ａ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 8)
A conductive pressure-sensitive adhesive sheet was produced in the same manner as in Example 1 except that the conductive pressure-sensitive adhesive composition (3A) was used instead of the conductive pressure-sensitive adhesive composition (1A-1).
（実施例９）
導電性粘着剤組成物（１Ａ−１）の代わりに、導電性粘着剤組成物（４Ａ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。Example 9
A conductive pressure-sensitive adhesive sheet was produced in the same manner as in Example 1 except that the conductive pressure-sensitive adhesive composition (4A) was used instead of the conductive pressure-sensitive adhesive composition (1A-1).
（実施例１０）
導電性粘着剤層の厚さを９μｍから７μｍに変更したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 10)
A conductive pressure-sensitive adhesive sheet was produced in the same manner as in Example 1 except that the thickness of the conductive pressure-sensitive adhesive layer was changed from 9 μm to 7 μm.
（実施例１１）
導電性粘着剤層の厚さを９μｍから１５μｍに変更したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 11)
A conductive pressure-sensitive adhesive sheet was produced in the same manner as in Example 1 except that the thickness of the conductive pressure-sensitive adhesive layer was changed from 9 μm to 15 μm.
（実施例１２）
導電性粘着剤組成物（１Ａ−１）の代わりに、導電性粘着剤組成物（１Ｂ）を使用し、かつ、導電性粘着剤層の厚さを９μｍから１８μｍに変更したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 12)
Implemented except that instead of the conductive adhesive composition (1A-1), the conductive adhesive composition (1B) was used and the thickness of the conductive adhesive layer was changed from 9 μm to 18 μm. A conductive pressure-sensitive adhesive sheet was produced in the same manner as in Example 1.
（実施例１３）
導電性粘着剤組成物（１Ａ−１）の代わりに、導電性粘着剤組成物（１Ｂ）を使用し、かつ、導電性粘着剤層の厚さを９μｍから１３μｍに変更したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 13)
Implemented except that instead of the conductive adhesive composition (1A-1), the conductive adhesive composition (1B) was used, and the thickness of the conductive adhesive layer was changed from 9 μm to 13 μm. A conductive pressure-sensitive adhesive sheet was produced in the same manner as in Example 1.
（実施例１４）
メッキ不織布Ａの代わりに、メッキ不織布Ｅを用いた以外は実施例１と同様に実施例１４の導電性粘着シートを作成した。(Example 14)
A conductive adhesive sheet of Example 14 was prepared in the same manner as Example 1 except that the plated nonwoven fabric E was used instead of the plated nonwoven fabric A.
（実施例１５）
導電性基材（Ａ）の代わりに、導電性基材（Ｆ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 15)
A conductive adhesive sheet was produced in the same manner as in Example 1 except that the conductive substrate (F) was used instead of the conductive substrate (A).
（実施例１６）
導電性基材（Ａ）の代わりに、導電性基材（Ｇ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 16)
A conductive adhesive sheet was produced in the same manner as in Example 1 except that the conductive substrate (G) was used instead of the conductive substrate (A).
（実施例１７）
導電性基材（Ａ）の代わりに、導電性基材（Ｈ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Example 17)
A conductive adhesive sheet was produced in the same manner as in Example 1 except that the conductive substrate (H) was used instead of the conductive substrate (A).
（比較例１）
導電性基材（Ａ）の代わりに、導電性基材（Ｉ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Comparative Example 1)
A conductive adhesive sheet was produced in the same manner as in Example 1 except that the conductive substrate (I) was used instead of the conductive substrate (A).
（比較例２）
導電性基材（Ａ）の代わりに、導電性基材（Ｊ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Comparative Example 2)
A conductive adhesive sheet was produced in the same manner as in Example 1 except that the conductive substrate (J) was used instead of the conductive substrate (A).
（比較例３）
導電性基材（Ａ）の代わりに、導電性基材（Ｋ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Comparative Example 3)
A conductive adhesive sheet was produced in the same manner as in Example 1 except that the conductive substrate (K) was used instead of the conductive substrate (A).
（比較例４）
導電性基材（Ａ）の代わりに、導電性基材（Ｌ）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Comparative Example 4)
A conductive adhesive sheet was produced in the same manner as in Example 1 except that the conductive substrate (L) was used instead of the conductive substrate (A).
（比較例５）
導電性粘着剤組成物（１Ａ−１）の代わりに、導電性粘着剤組成物（１Ａ−４）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Comparative Example 5)
A conductive pressure-sensitive adhesive sheet was produced in the same manner as in Example 1 except that the conductive pressure-sensitive adhesive composition (1A-4) was used instead of the conductive pressure-sensitive adhesive composition (1A-1).
（比較例６）
導電性粘着剤組成物（１Ａ−１）の代わりに、導電性粘着剤組成物（１Ａ−５）を使用したこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Comparative Example 6)
A conductive pressure-sensitive adhesive sheet was produced in the same manner as in Example 1 except that the conductive pressure-sensitive adhesive composition (1A-5) was used instead of the conductive pressure-sensitive adhesive composition (1A-1).
（参考例１）
導電性基材（Ａ）の代わりに、厚さ９μｍの無機防錆（クロメート）処理した電解銅箔（ＣＦ−Ｔ９ＦＺ−ＳＶ、福田金属箔粉工業社製）を用いたこと以外は、実施例１と同様の方法で導電性粘着シートを作製した。(Reference Example 1)
Except for using an electro-conductive copper foil (CF-T9FZ-SV, manufactured by Fukuda Metal Foil Powder Industry Co., Ltd.) having a thickness of 9 μm treated with inorganic rust prevention (chromate) instead of the conductive substrate (A). A conductive adhesive sheet was prepared in the same manner as in 1.
前記導電性基材、導電性粘着剤層及び導電性粘着シートについて、以下の評価を行い、得られた結果を下表に示した。なお、表中のアクリル酸量は、アクリル系共重合体の製造に使用した単量体成分の全量に対するアクリル酸の使用量（質量％）を表す。また、表中の金属粉量は導電性粘着剤層の全体に対する導電性粒子の含有量（質量％）を表す。また、実施例１及び参考例１の追従性評価結果を図３及び図４に示した。 The following evaluation was performed about the said conductive base material, a conductive adhesive layer, and a conductive adhesive sheet, and the obtained result was shown to the following table. In addition, the acrylic acid amount in a table | surface represents the usage-amount (mass%) of acrylic acid with respect to the whole quantity of the monomer component used for manufacture of an acryl-type copolymer. Moreover, the amount of metal powder in the table represents the content (% by mass) of conductive particles with respect to the entire conductive adhesive layer. Moreover, the follow-up evaluation results of Example 1 and Reference Example 1 are shown in FIGS.
［粒子径］
導電性粒子の粒子径は、株式会社島津製作所製のレーザー回折式粒度分布測定器ＳＡＬＤ−３０００を用い、分散媒にイソプロパノールを使用して測定した値を指す。[Particle size]
The particle diameter of the conductive particles refers to a value measured using a laser diffraction particle size distribution analyzer SALD-3000 manufactured by Shimadzu Corporation and using isopropanol as a dispersion medium.
［導電性（導電性粘着シート）］
３０ｍｍ幅×３０ｍｍ幅の導電性粘着シートの一方の面を２５ｍｍ×２５ｍｍの真鍮製電極に貼り付けた。導電性粘着シートのもう一方の面に３０ｍｍ×８０ｍｍの銅箔（厚さ３５μｍ）を貼り付けた。[Conductivity (conductive adhesive sheet)]
One surface of a 30 mm wide × 30 mm wide conductive adhesive sheet was attached to a 25 mm × 25 mm brass electrode. A 30 mm × 80 mm copper foil (thickness: 35 μm) was attached to the other surface of the conductive adhesive sheet.
前記真鍮製電極の上から面圧２０Ｎの荷重をかけた状態で、前記真鍮製電極と前記銅箔とに端子を接続し、２３℃及び５０％ＲＨの環境下、ミリオームメーター（エヌエフ回路設計製）を用い１０μＡの電流を流した際の抵抗値を測定した。前記抵抗値が５００ｍΩ以下である場合を合格とした。 A terminal is connected to the brass electrode and the copper foil with a surface pressure of 20 N applied from above the brass electrode, and a milliohm meter (manufactured by NF Circuit Design Co., Ltd.) in an environment of 23 ° C. and 50% RH. ) Was used to measure the resistance value when a current of 10 μA was passed. The case where the resistance value was 500 mΩ or less was regarded as acceptable.
［厚さ（導電性粘着剤層）］
各導電性粘着剤組成物を用いて剥離フィルム上に形成された導電性粘着剤層に、ＰＥＴフィルム２５μｍ（ユニチカ社製Ｓ２５）を裏打ちした試料を作成し、その厚さをテスター産業社製の厚さ計「ＴＨ−１０２」を用いて測定した。前記測定値から、前記剥離フィルム及びＰＥＴフィルムの厚さを減じた値を導電性粘着剤層の厚さとした。[Thickness (conductive adhesive layer)]
Using a conductive pressure-sensitive adhesive layer formed on a release film using each conductive pressure-sensitive adhesive composition, a sample lined with a PET film 25 μm (S25 manufactured by Unitika Co., Ltd.) was prepared, and the thickness was made by Tester Sangyo Co., Ltd. It was measured using a thickness meter “TH-102”. The value obtained by subtracting the thickness of the release film and the PET film from the measured value was defined as the thickness of the conductive adhesive layer.
［厚さ（導電性粘着シート）］
テスター産業社製の厚さ計「ＴＨ−１０２」を用い導電性粘着シートの厚さを測定した。[Thickness (conductive adhesive sheet)]
The thickness of the conductive adhesive sheet was measured using a thickness meter “TH-102” manufactured by Tester Sangyo Co., Ltd.
［導電性（導電性基材）］
３０ｍｍ幅×３０ｍｍ幅の導電性基材を、二つの２５ｍｍ×２５ｍｍの真鍮製電極に挟み込み、真鍮製電極の上から面圧２０Ｎの荷重をかけた状態で、各真鍮製電極に端子を接続し、２３℃及び５０％ＲＨの環境下、ミリオームメーター（エヌエフ回路設計製）を用い１０μＡの電流を流した際の抵抗値を測定した。[Conductivity (conductive substrate)]
A conductive base material of 30 mm width × 30 mm width is sandwiched between two brass electrodes of 25 mm × 25 mm, and a terminal is connected to each brass electrode with a surface pressure of 20 N applied from above the brass electrode. The resistance value when a current of 10 μA was passed was measured using a milliohm meter (manufactured by NF Circuit Design) in an environment of 23 ° C. and 50% RH.
［接着力］
２０ｍｍ幅の導電性粘着シートを用意し、一方の面を厚さ２５μｍのポリエチレンテレフタレートフィルム（ユニチカ株式会社製Ｓ２５）を用い裏打ちしたものを試験片とした。[Adhesive strength]
A conductive adhesive sheet having a width of 20 mm was prepared, and a test piece was prepared by lining one surface with a polyethylene terephthalate film (S25 manufactured by Unitika Ltd.) having a thickness of 25 μm.
次に、２３℃及び５０％ＲＨの環境下、３６０番の耐水研磨紙を用いてヘアライン研磨処理したステンレス板（以下ステンレス板）に、前記試験片の粘着剤層を貼付し、その上面から２．０ｋｇローラーを１往復させることでそれらを圧着させた。 Next, the pressure-sensitive adhesive layer of the test piece was attached to a stainless steel plate (hereinafter referred to as a stainless steel plate) subjected to hairline polishing treatment using No. 360 water-resistant abrasive paper in an environment of 23 ° C. and 50% RH. They were crimped by reciprocating a 0 kg roller once.
次に、前記圧着したものを常温下に１時間放置した後、引っ張り試験機（テンシロンＲＴＡ−１００、エーアンドディー社製）を用い、常温で引張速度３００ｍｍ／ｍｉｎで試験することによって１８０度剥離接着力を測定した。上記接着力の試験を、導電性粘着シートの各粘着剤層（両面の粘着剤層）に対して行い、低い方の値を表に記載した。 Next, the pressure-bonded product is allowed to stand at room temperature for 1 hour and then peeled 180 degrees by testing at a normal temperature and a tensile speed of 300 mm / min using a tensile tester (Tensilon RTA-100, manufactured by A & D). The adhesive force was measured. The test of the said adhesive force was performed with respect to each adhesive layer (double-sided adhesive layer) of an electroconductive adhesive sheet, and the lower value was described in the table | surface.
[追従性]
深さ５ｍｍ及び幅１０ｍｍの略半円型の段差を有する金属板に、導電性粘着シートを手で貼付け、段差への追従性を評価した。[Followability]
A conductive adhesive sheet was attached by hand to a metal plate having a substantially semicircular step having a depth of 5 mm and a width of 10 mm, and the followability to the step was evaluated.
○：段差に追従できた。 ○: Following the step.
×：段差に追従できず、浮き又は破れが生じた。 X: Unable to follow the step and floated or torn.
［リワーク性１］
前記方法で接着力を測定した際にステンレス板への糊残りの有無を評価した。[Reworkability 1]
When the adhesive force was measured by the above method, the presence or absence of adhesive residue on the stainless steel plate was evaluated.
◎：糊残りなし。 A: No adhesive residue.
○：ステンレス板の面積に対し１０％未満の範囲に糊残りがあった。 ○: There was adhesive residue in a range of less than 10% with respect to the area of the stainless steel plate.
×：ステンレス板の面積に対し１０％以上の範囲に糊残りがあった。 X: The adhesive residue was in the range of 10% or more with respect to the area of the stainless steel plate.
［リワーク性２］
前記方法で接着力を測定した際に、導電性粘着シートが破れるか否かを評価した。５つの導電性粘着シートを用いて試験を実施し、下記基準にて評価した。[Reworkability 2]
When the adhesive force was measured by the above method, it was evaluated whether or not the conductive adhesive sheet was torn. The test was carried out using five conductive adhesive sheets, and the following criteria were evaluated.
◎：５個ともヤブレなし。 A: No blurring on all five.
○：４個ヤブレなし。 ◯: No 4 blurs.
×：２個以上ヤブレが発生。 X: Two or more jabbing occurred.
上記表から明らかなとおり、本願発明の実施例１〜１８の粘着シートは、追従性に優れ、かつ接着性、導電性、リワーク性も良好であった。一方、比較例１〜４の粘着シートは、追従性、導電性、接着性に優れるものの、著しくリワーク性に劣っていた。比較例５の粘着シートは導電性に劣っていた。比較例６の粘着シートは接着性、リワーク性に劣っていた。また参考例の粘着シートは追従性に劣っており、段差部にて浮き及び破れが生じた。 As is clear from the above table, the pressure-sensitive adhesive sheets of Examples 1 to 18 of the present invention were excellent in followability, and had good adhesion, conductivity, and reworkability. On the other hand, although the adhesive sheet of Comparative Examples 1-4 was excellent in followability, electroconductivity, and adhesiveness, it was inferior to rework property remarkably. The pressure-sensitive adhesive sheet of Comparative Example 5 was inferior in conductivity. The pressure-sensitive adhesive sheet of Comparative Example 6 was inferior in adhesiveness and reworkability. Further, the pressure-sensitive adhesive sheet of the reference example was inferior in followability, and floated and torn at the step portion.
１ 導電性基材
２ 導電性粘着剤層1
Claims (14)
前記導電性基材が、湿式ポリエステル系不織布基材に、無電解メッキ処理を含むメッキ処理を施すことによって得られたものであり、
前記導電性粘着剤層が、前記導電性粘着剤層全体に対して導電性粒子を３質量％〜５０質量％含有するものであることを特徴とする導電性粘着シート。A conductive pressure-sensitive adhesive sheet having a conductive pressure-sensitive adhesive layer on at least one surface of a conductive substrate,
The conductive substrate is obtained by subjecting a wet polyester nonwoven fabric substrate to a plating treatment including an electroless plating treatment,
The conductive pressure-sensitive adhesive sheet, wherein the conductive pressure-sensitive adhesive layer contains 3% by mass to 50% by mass of conductive particles with respect to the entire conductive pressure-sensitive adhesive layer.
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| WO2017061597A1 (en) * | 2015-10-07 | 2017-04-13 | 積水化学工業株式会社 | Metal-coated nonwoven fabric with adhesive layer, process for producing metal-coated nonwoven fabric with adhesive layer, and covered core wire |
| JP6660542B2 (en) | 2015-11-30 | 2020-03-11 | タツタ電線株式会社 | Stretchable conductive film for textile |
| JPWO2017170371A1 (en) * | 2016-03-30 | 2019-02-07 | 積水化学工業株式会社 | Conductive adhesive tape |
| JP6930239B2 (en) * | 2017-06-15 | 2021-09-01 | Dic株式会社 | Conductive adhesive sheet |
| JP6996121B2 (en) * | 2017-06-16 | 2022-01-17 | Dic株式会社 | Conductive adhesive sheet |
| JP6969172B2 (en) * | 2017-06-16 | 2021-11-24 | Dic株式会社 | Conductive adhesive sheet |
| JP6914796B2 (en) * | 2017-09-28 | 2021-08-04 | 信越ポリマー株式会社 | Silicone rubber composition for concrete surface covering member, concrete surface covering member and concrete surface covering method using it |
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| JP4403360B2 (en) | 2003-02-28 | 2010-01-27 | Ｄｉｃ株式会社 | Conductive adhesive sheet |
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