TW202405117A - adhesive sheet - Google Patents
adhesive sheet Download PDFInfo
- Publication number
- TW202405117A TW202405117A TW112115305A TW112115305A TW202405117A TW 202405117 A TW202405117 A TW 202405117A TW 112115305 A TW112115305 A TW 112115305A TW 112115305 A TW112115305 A TW 112115305A TW 202405117 A TW202405117 A TW 202405117A
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- TW
- Taiwan
- Prior art keywords
- mass
- monomer
- meth
- polymer
- mentioned
- Prior art date
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- 239000000853 adhesive Substances 0.000 title claims abstract description 173
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 173
- 239000000178 monomer Substances 0.000 claims abstract description 218
- 229920000642 polymer Polymers 0.000 claims abstract description 101
- 239000012790 adhesive layer Substances 0.000 claims abstract description 76
- 229910052751 metal Inorganic materials 0.000 claims abstract description 50
- 239000002184 metal Substances 0.000 claims abstract description 50
- 239000000463 material Substances 0.000 claims abstract description 36
- 125000000524 functional group Chemical group 0.000 claims abstract description 33
- 239000002530 phenolic antioxidant Substances 0.000 claims abstract description 28
- 230000009477 glass transition Effects 0.000 claims abstract description 23
- 229920001519 homopolymer Polymers 0.000 claims abstract description 22
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000000758 substrate Substances 0.000 claims description 23
- 150000001875 compounds Chemical class 0.000 claims description 13
- 239000011149 active material Substances 0.000 claims description 3
- -1 acrylate Pentyl ester Chemical class 0.000 description 71
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 63
- 229920005989 resin Polymers 0.000 description 40
- 239000011347 resin Substances 0.000 description 40
- 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 38
- 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 38
- 239000003431 cross linking reagent Substances 0.000 description 38
- 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 38
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 35
- 239000003999 initiator Substances 0.000 description 30
- 229920000058 polyacrylate Polymers 0.000 description 29
- 150000003505 terpenes Chemical class 0.000 description 24
- 235000007586 terpenes Nutrition 0.000 description 23
- 239000000203 mixture Substances 0.000 description 21
- 239000007789 gas Substances 0.000 description 20
- 238000006116 polymerization reaction Methods 0.000 description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 16
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 16
- 150000002430 hydrocarbons Chemical group 0.000 description 16
- 238000000034 method Methods 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 15
- 239000011889 copper foil Substances 0.000 description 14
- 125000000217 alkyl group Chemical group 0.000 description 13
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- 239000003505 polymerization initiator Substances 0.000 description 13
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 12
- 125000004433 nitrogen atom Chemical group N* 0.000 description 12
- 150000002978 peroxides Chemical class 0.000 description 12
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 11
- 239000005011 phenolic resin Substances 0.000 description 11
- 239000000523 sample Substances 0.000 description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- 150000002148 esters Chemical class 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- 229920002554 vinyl polymer Polymers 0.000 description 10
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 9
- 238000004132 cross linking Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 125000001931 aliphatic group Chemical group 0.000 description 8
- 239000003963 antioxidant agent Substances 0.000 description 8
- 235000006708 antioxidants Nutrition 0.000 description 8
- 239000011888 foil Substances 0.000 description 8
- 239000012948 isocyanate Substances 0.000 description 8
- 239000010410 layer Substances 0.000 description 8
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 8
- 238000010943 off-gassing Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 150000003926 acrylamides Chemical class 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- 150000002513 isocyanates Chemical class 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- GRWFGVWFFZKLTI-IUCAKERBSA-N (-)-α-pinene Chemical compound CC1=CC[C@@H]2C(C)(C)[C@H]1C2 GRWFGVWFFZKLTI-IUCAKERBSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 6
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 6
- 239000012986 chain transfer agent Substances 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 125000000962 organic group Chemical group 0.000 description 6
- 239000005056 polyisocyanate Substances 0.000 description 6
- 229920001228 polyisocyanate Polymers 0.000 description 6
- 230000003595 spectral effect Effects 0.000 description 6
- 238000012719 thermal polymerization Methods 0.000 description 6
- WDQMWEYDKDCEHT-UHFFFAOYSA-N 2-ethylhexyl 2-methylprop-2-enoate Chemical compound CCCCC(CC)COC(=O)C(C)=C WDQMWEYDKDCEHT-UHFFFAOYSA-N 0.000 description 5
- 239000004593 Epoxy Substances 0.000 description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 5
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 5
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 5
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 5
- 125000002723 alicyclic group Chemical group 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 238000005227 gel permeation chromatography Methods 0.000 description 5
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 5
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 4
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 4
- 239000012965 benzophenone Substances 0.000 description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000012943 hotmelt Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- 239000005020 polyethylene terephthalate Substances 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 4
- WTARULDDTDQWMU-RKDXNWHRSA-N (+)-β-pinene Chemical compound C1[C@H]2C(C)(C)[C@@H]1CCC2=C WTARULDDTDQWMU-RKDXNWHRSA-N 0.000 description 3
- WTARULDDTDQWMU-IUCAKERBSA-N (-)-Nopinene Natural products C1[C@@H]2C(C)(C)[C@H]1CCC2=C WTARULDDTDQWMU-IUCAKERBSA-N 0.000 description 3
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical class O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 3
- GAVHQOUUSHBDAA-UHFFFAOYSA-N 3-butyl-1-ethenylaziridin-2-one Chemical compound CCCCC1N(C=C)C1=O GAVHQOUUSHBDAA-UHFFFAOYSA-N 0.000 description 3
- QRLSTWVLSWCGBT-UHFFFAOYSA-N 4-((4,6-bis(octylthio)-1,3,5-triazin-2-yl)amino)-2,6-di-tert-butylphenol Chemical compound CCCCCCCCSC1=NC(SCCCCCCCC)=NC(NC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=N1 QRLSTWVLSWCGBT-UHFFFAOYSA-N 0.000 description 3
- OSJIQLQSJBXTOH-UHFFFAOYSA-N 8-tricyclo[5.2.1.02,6]decanylmethyl prop-2-enoate Chemical compound C12CCCC2C2CC(COC(=O)C=C)C1C2 OSJIQLQSJBXTOH-UHFFFAOYSA-N 0.000 description 3
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 3
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- WTARULDDTDQWMU-UHFFFAOYSA-N Pseudopinene Natural products C1C2C(C)(C)C1CCC2=C WTARULDDTDQWMU-UHFFFAOYSA-N 0.000 description 3
- 244000028419 Styrax benzoin Species 0.000 description 3
- 235000000126 Styrax benzoin Nutrition 0.000 description 3
- 235000008411 Sumatra benzointree Nutrition 0.000 description 3
- 239000007983 Tris buffer Substances 0.000 description 3
- XCPQUQHBVVXMRQ-UHFFFAOYSA-N alpha-Fenchene Natural products C1CC2C(=C)CC1C2(C)C XCPQUQHBVVXMRQ-UHFFFAOYSA-N 0.000 description 3
- MVNCAPSFBDBCGF-UHFFFAOYSA-N alpha-pinene Natural products CC1=CCC23C1CC2C3(C)C MVNCAPSFBDBCGF-UHFFFAOYSA-N 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 239000007869 azo polymerization initiator Substances 0.000 description 3
- 229960002130 benzoin Drugs 0.000 description 3
- 229930006722 beta-pinene Natural products 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 3
- 125000005442 diisocyanate group Chemical group 0.000 description 3
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- LCWMKIHBLJLORW-UHFFFAOYSA-N gamma-carene Natural products C1CC(=C)CC2C(C)(C)C21 LCWMKIHBLJLORW-UHFFFAOYSA-N 0.000 description 3
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 3
- 235000019382 gum benzoic Nutrition 0.000 description 3
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- 150000002894 organic compounds Chemical class 0.000 description 3
- 229920001568 phenolic resin Polymers 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 230000000379 polymerizing effect Effects 0.000 description 3
- GRWFGVWFFZKLTI-UHFFFAOYSA-N rac-alpha-Pinene Natural products CC1=CCC2C(C)(C)C1C2 GRWFGVWFFZKLTI-UHFFFAOYSA-N 0.000 description 3
- 229930195734 saturated hydrocarbon Natural products 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical class CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 3
- XMGQYMWWDOXHJM-JTQLQIEISA-N (+)-α-limonene Chemical compound CC(=C)[C@@H]1CCC(C)=CC1 XMGQYMWWDOXHJM-JTQLQIEISA-N 0.000 description 2
- RTTZISZSHSCFRH-UHFFFAOYSA-N 1,3-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC(CN=C=O)=C1 RTTZISZSHSCFRH-UHFFFAOYSA-N 0.000 description 2
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 2
- OZFIGURLAJSLIR-UHFFFAOYSA-N 1-ethenyl-2h-pyridine Chemical compound C=CN1CC=CC=C1 OZFIGURLAJSLIR-UHFFFAOYSA-N 0.000 description 2
- STFXXRRQKFUYEU-UHFFFAOYSA-N 16-methylheptadecyl prop-2-enoate Chemical compound CC(C)CCCCCCCCCCCCCCCOC(=O)C=C STFXXRRQKFUYEU-UHFFFAOYSA-N 0.000 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 2
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 description 2
- BVUXDWXKPROUDO-UHFFFAOYSA-N 2,6-di-tert-butyl-4-ethylphenol Chemical compound CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 BVUXDWXKPROUDO-UHFFFAOYSA-N 0.000 description 2
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 description 2
- NLGDWWCZQDIASO-UHFFFAOYSA-N 2-hydroxy-1-(7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-yl)-2-phenylethanone Chemical compound OC(C(=O)c1cccc2Oc12)c1ccccc1 NLGDWWCZQDIASO-UHFFFAOYSA-N 0.000 description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
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- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 description 1
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- 229960000984 tocofersolan Drugs 0.000 description 1
- RUELTTOHQODFPA-UHFFFAOYSA-N toluene 2,6-diisocyanate Chemical compound CC1=C(N=C=O)C=CC=C1N=C=O RUELTTOHQODFPA-UHFFFAOYSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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Classifications
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- B32B27/00—Layered products comprising a layer of synthetic resin
-
- 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
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- C—CHEMISTRY; METALLURGY
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- C09J11/08—Macromolecular additives
-
- 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
- C09J201/00—Adhesives based on unspecified macromolecular compounds
-
- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/28—Metal sheet
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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
- 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
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- H—ELECTRICITY
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- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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- H01M4/00—Electrodes
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- H01M4/64—Carriers or collectors
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
-
- 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
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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
- C09J143/00—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 containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Adhesives based on derivatives of such polymers
- C09J143/04—Homopolymers or copolymers of monomers containing silicon
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
Description
本發明係關於一種黏著片材。The present invention relates to an adhesive sheet.
作為以移動式機器為代表之電子機器之電源而迅速發展之鋰電池於EV車(Electric Vehicle,電力車)中亦得到實際應用。EV車之當務之急除負載重量以外,還迫切需要解決使用時之變形(膨脹)或著火等由電池所含有之電解液引起之問題。因此,近數年間,全固體電池之普及備受期待,而於該電池之電路零件固定用途等方面,使用黏著片材(黏著帶)。要求此種黏著片材之導電性優異。Lithium batteries, which are rapidly developing as power sources for electronic equipment represented by mobile machines, are also being used in EV vehicles (Electric Vehicles). In addition to the load capacity, the top priority for EV vehicles is also the urgent need to solve problems caused by the electrolyte contained in the battery, such as deformation (expansion) or fire during use. Therefore, in recent years, the popularization of all-solid-state batteries has been highly anticipated, and adhesive sheets (adhesive tapes) are used for fixing circuit parts of such batteries. The adhesive sheet is required to have excellent electrical conductivity.
又,黏著片材若自接著初期起黏著力便較高,則難以重新貼附,因此就初始黏著力較弱,但可將被黏著體牢固地固定之方面而言,謀求一種黏著力隨時間上升,且可獲得較高之黏著力之黏著片材。In addition, if the adhesive sheet has a high adhesive force from the initial stage of adhesion, it will be difficult to reattach it. Therefore, the initial adhesive force is weak but the adherend can be firmly fixed. It is necessary to seek an adhesive force that changes over time. rise, and can obtain adhesive sheets with higher adhesion.
專利文獻1中揭示一種黏著劑組合物,該黏著劑組合物可形成一種初始黏著力較弱,可輕易自被黏著體剝離即二次加工性優異,且黏著力隨時間上升之黏著劑層。 先前技術文獻 專利文獻 Patent Document 1 discloses an adhesive composition that can form an adhesive layer that has a weak initial adhesive force, can be easily peeled off from an adherend, has excellent secondary processability, and has an adhesive force that increases with time. Prior technical literature patent documents
專利文獻1:日本專利特開2014-224227號公報Patent Document 1: Japanese Patent Application Publication No. 2014-224227
[發明所欲解決之問題][Problem to be solved by the invention]
就環境保護之觀點、或防止因引火所導致之著火等之觀點而言,要求全固體電池之電路零件固定用黏著片材之釋氣量較少。From the viewpoint of environmental protection or the prevention of ignition caused by ignition, adhesive sheets for fixing circuit components of all-solid-state batteries are required to have a small amount of outgassing.
本發明係鑒於此種情況而想出者,其目的在於提供一種導電性及二次加工性優異,黏著力隨時間上升,且釋氣量較少之黏著片材。 [解決問題之技術手段] The present invention was conceived in view of this situation, and its purpose is to provide an adhesive sheet that is excellent in conductivity and secondary processability, has an adhesive force that increases with time, and has a small amount of outgassing. [Technical means to solve problems]
本發明人等為了達成上述目的而銳意研究,結果發現具備金屬基材及設置於其至少一面之特定之黏著劑層的黏著片材之導電性及二次加工性優異,黏著力隨時間上升,且釋氣量較少。本發明係基於該等見解所完成者。The inventors of the present invention conducted intensive research to achieve the above object, and found that an adhesive sheet having a metal base material and a specific adhesive layer provided on at least one side of the adhesive sheet has excellent electrical conductivity and secondary processability, and the adhesive force increases with time. And the amount of gas released is less. The present invention was completed based on these findings.
即,本發明提供一種黏著片材,其具備:金屬基材、及設置於上述金屬基材之至少一面之黏著劑層,且 上述黏著劑層相對於玻璃轉移溫度未達0℃之聚合物(A)100質量份,包含聚合物(B)0.1~20質量份、及酚系抗氧化劑0.4質量份以上,該聚合物(B)包含具有聚有機矽氧烷骨架之單體(B1)及均聚物之玻璃轉移溫度為40℃以上之單體(B2)作為單體單元,並且單體(B1)之官能基當量(算術平均)為1000 g/mol以上且未達15000 g/mol,且該聚合物(B)之重量平均分子量為10000以上且未達100000。 That is, the present invention provides an adhesive sheet including a metal base material and an adhesive layer provided on at least one side of the metal base material, and The above-mentioned adhesive layer contains 0.1 to 20 parts by mass of polymer (B) and more than 0.4 parts by mass of phenolic antioxidant relative to 100 parts by mass of polymer (A) whose glass transition temperature is less than 0°C. The polymer (B) ) contains a monomer (B1) with a polyorganosiloxane skeleton and a monomer (B2) with a homopolymer glass transition temperature of 40°C or above as monomer units, and the functional group equivalent of the monomer (B1) (arithmetic average) is 1000 g/mol or more and less than 15000 g/mol, and the weight average molecular weight of the polymer (B) is 10000 or more but less than 100000.
上述酚系抗氧化劑較佳為包含具有2個以上之酚骨架之化合物。The phenolic antioxidant preferably contains a compound having two or more phenolic skeletons.
上述黏著片材之總釋氣量較佳為15500 ppm以下。The total gas release amount of the above-mentioned adhesive sheet is preferably less than 15500 ppm.
上述黏著片材較佳為用於電池構件貼附用途。The above-mentioned adhesive sheet is preferably used for attaching battery components.
上述黏著片材較佳為用於全固體電池構件貼附用途。The above-mentioned adhesive sheet is preferably used for attaching all-solid-state battery components.
又,本發明提供一種全固體電池用電極,其具備:絕緣基板、上述黏著劑層貼合於上述絕緣基板而成之上述黏著片材、及附著於上述黏著片材中之金屬基材之活性物質。 [發明之效果] Furthermore, the present invention provides an electrode for an all-solid-state battery, which includes an insulating substrate, the adhesive sheet in which the adhesive layer is bonded to the insulating substrate, and the activity of a metal base material adhered to the adhesive sheet. material. [Effects of the invention]
本發明之黏著片材之導電性及二次加工性優異,黏著力隨時間上升,且釋氣量較少。因此,上述黏著片材適宜用於全固體電池之電路零件固定用途,又,此時所產生之釋氣量較少,因此不易因引火而導致著火等。The adhesive sheet of the present invention has excellent electrical conductivity and secondary processability, the adhesive force increases with time, and the amount of gas release is small. Therefore, the above-mentioned adhesive sheet is suitable for fixing circuit parts of all-solid-state batteries. In addition, the amount of outgassing generated at this time is small, so it is less likely to cause fire due to ignition.
<黏著片材> 本發明之黏著片材至少具備:金屬基材、及設置於上述金屬基材之至少一面之黏著劑層。本發明之黏著片材可為雙面均成為黏著劑層表面之雙面黏著片材,亦可為僅單面成為黏著劑層表面之單面黏著片材。 <Adhesive sheet> The adhesive sheet of the present invention at least includes a metal base material and an adhesive layer provided on at least one side of the metal base material. The adhesive sheet of the present invention may be a double-sided adhesive sheet in which both sides become the surface of the adhesive layer, or may be a single-sided adhesive sheet in which only one side becomes the surface of the adhesive layer.
圖1係表示本發明之黏著片材之一實施方式之剖視模式圖。如圖1所示,黏著片材1係具備金屬基材2、及設置於金屬基材2之其中一面之黏著劑層3的單面黏著片材。FIG. 1 is a schematic cross-sectional view showing one embodiment of the adhesive sheet of the present invention. As shown in FIG. 1 , the adhesive sheet 1 is a single-sided adhesive sheet including a metal base material 2 and an adhesive layer 3 provided on one side of the metal base material 2 .
[金屬基材] 上述金屬基材較佳為沿面方向延伸之金屬箔。上述金屬基材可為單層,亦可為複數層。於複數層之情形時,各層之構成金屬或厚度等可相同,亦可不同。 [Metal base material] The above-mentioned metal substrate is preferably a metal foil extending in the surface direction. The above-mentioned metal substrate may be a single layer or multiple layers. In the case of multiple layers, the constituent metal or thickness of each layer may be the same or different.
作為構成上述金屬基材之金屬,例如可例舉:銅、鋁、金、鎳、鈦、鉬、鈮、鉭、鋯、合金等。作為上述合金,例如可例舉:不鏽鋼、鎳鐵合金、鎳鉻合金等。作為上述金屬,就可獲得優異之導電性之觀點而言,較佳為銅。即,上述金屬基材較佳為銅箔。Examples of the metal constituting the metal base material include copper, aluminum, gold, nickel, titanium, molybdenum, niobium, tantalum, zirconium, alloys, and the like. Examples of the alloy include stainless steel, nickel-iron alloy, nickel-chromium alloy, and the like. As the above-mentioned metal, copper is preferred from the viewpoint of obtaining excellent electrical conductivity. That is, the metal base material is preferably copper foil.
上述金屬基材之形成方法並無特別限定,例如可例舉:電解、蒸鍍(例如真空蒸鍍)、濺鍍、CVD(chemical vapor deposition,化學氣相沈積)法、金屬有機(MO)、鍍覆、壓延加工等。The formation method of the above-mentioned metal substrate is not particularly limited. For example, electrolysis, evaporation (such as vacuum evaporation), sputtering, CVD (chemical vapor deposition, chemical vapor deposition) method, metal-organic (MO), Plating, rolling processing, etc.
上述金屬基材之厚度例如為1 μm以上,較佳為5 μm以上,更佳為10 μm以上,進而較佳為15 μm以上。上述厚度例如為300 μm以下,較佳為200 μm以下,更佳為100 μm以下,進而較佳為80 μm以下,特佳為50 μm以下。The thickness of the metal substrate is, for example, 1 μm or more, preferably 5 μm or more, more preferably 10 μm or more, and further preferably 15 μm or more. The thickness is, for example, 300 μm or less, preferably 200 μm or less, more preferably 100 μm or less, further preferably 80 μm or less, particularly preferably 50 μm or less.
[黏著劑層] 上述黏著劑層至少包含:聚合物(A)、聚合物(B)、及酚系抗氧化劑。藉由使用此種黏著劑層,可將本發明之黏著片材製成對被黏著體之初始黏著力較低而二次加工性優異,且黏著力隨時間上升,對被黏著體之黏著性優異之黏著片材。 [Adhesive layer] The above-mentioned adhesive layer contains at least: polymer (A), polymer (B), and phenolic antioxidant. By using this adhesive layer, the adhesive sheet of the present invention can be made to have low initial adhesive force to the adherend and excellent secondary processability, and the adhesive force increases with time, and the adhesiveness to the adherend is improved. Excellent adhesive sheet.
上述黏著劑層相對於聚合物(A)100質量份,包含聚合物(B)0.1~20質量份、及酚系抗氧化劑0.4質量份以上。再者,於本說明書中,有時將上述黏著劑層稱為「本發明之黏著劑層」。The above-mentioned adhesive layer contains 0.1 to 20 parts by mass of polymer (B) and 0.4 or more parts by mass of phenolic antioxidant based on 100 parts by mass of polymer (A). Furthermore, in this specification, the above-mentioned adhesive layer may be referred to as "the adhesive layer of the present invention".
本發明之黏著片材可為雙面黏著片材,亦可為單面黏著片材。於本發明之黏著片材具備複數個黏著劑層之情形時,至少一個黏著劑層為本發明之黏著劑層,較佳為全部黏著劑層均為本發明之黏著劑層。又,複數個黏著劑層可相同,亦可為組成、厚度、物性等不同之黏著劑層。The adhesive sheet of the present invention can be a double-sided adhesive sheet or a single-sided adhesive sheet. When the adhesive sheet of the present invention has multiple adhesive layers, at least one adhesive layer is the adhesive layer of the present invention, and preferably all the adhesive layers are the adhesive layers of the present invention. In addition, the plurality of adhesive layers may be the same, or may be adhesive layers with different compositions, thicknesses, physical properties, etc.
(聚合物(A)) 聚合物(A)係玻璃轉移溫度未達0℃之聚合物。藉由使上述黏著劑層包含此種聚合物(A),而經時後仍能夠對被黏著體發揮出充分之黏著力。 (Polymer(A)) Polymer (A) is a polymer whose glass transition temperature is less than 0°C. By including the polymer (A) in the adhesive layer, sufficient adhesion to the adherend can still be exerted over time.
作為聚合物(A),例如可例舉:丙烯酸系聚合物、橡膠系聚合物、矽酮系聚合物、聚胺基甲酸酯系聚合物、聚酯系聚合物等作為黏著劑習用之各種聚合物。尤其是於聚合物(B)為(甲基)丙烯酸系聚合物之情形時,較佳為易於與(甲基)丙烯酸系聚合物相容而透明性較高之丙烯酸系聚合物。聚合物(A)可僅使用一種,亦可使用兩種以上。Examples of the polymer (A) include acrylic polymers, rubber polymers, silicone polymers, polyurethane polymers, polyester polymers and the like that are commonly used as adhesives. polymer. Especially when the polymer (B) is a (meth)acrylic polymer, an acrylic polymer that is easily compatible with the (meth)acrylic polymer and has high transparency is preferred. Only one type of polymer (A) may be used, or two or more types may be used.
聚合物(A)之玻璃轉移溫度(Tg)未達0℃,較佳為未達-10℃,更佳為未達-30℃。又,上述玻璃轉移溫度較佳為-80℃以上。若聚合物(A)之Tg為0℃以上,則存在聚合物不易流動,黏著力不易隨時間上升之情況。The glass transition temperature (Tg) of the polymer (A) is less than 0°C, preferably less than -10°C, more preferably less than -30°C. Moreover, it is preferable that the said glass transition temperature is -80 degreeC or more. If the Tg of the polymer (A) is 0° C. or higher, the polymer may not flow easily and the adhesive force may not easily increase with time.
玻璃轉移溫度為文獻、目錄等所記載之標稱值,或者為基於下述式(X)(Fox式)進行計算所得之值。 1/Tg=W 1/Tg 1+W 2/Tg 2+…+W n/Tg n(X) [於式(X)中,Tg表示聚合物(A)之玻璃轉移溫度(單位:K),Tg i(i=1、2、…n)表示單體i形成均聚物時之玻璃轉移溫度(單位:K),W i(i=1、2、…n)表示單體i於全部單體成分中之質量分率] 上述式(X)係聚合物(A)由單體1、單體2、…、單體n這n種單體成分構成時之計算式。 The glass transition temperature is a nominal value described in literature, catalogs, etc., or a value calculated based on the following formula (X) (Fox formula). 1/Tg=W 1 /Tg 1 +W 2 /Tg 2 +…+W n /Tg n (X) [In formula (X), Tg represents the glass transition temperature (unit: K) of polymer (A), Tg i (i=1, 2,...n) represents the glass transition temperature (unit: K) of monomer i when it forms a homopolymer, Wi ( i =1, 2,...n) represents monomer i among all monomers Mass fraction in components] The above formula (X) is a calculation formula when the polymer (A) is composed of n types of monomer components: monomer 1, monomer 2, ..., and monomer n.
再者,本說明書中之「形成均聚物時之玻璃轉移溫度(Tg)」(有時簡稱為「均聚物之Tg」)意指「該單體之均聚物之玻璃轉移溫度(Tg)」,具體而言,可例舉「Polymer Handbook」(第3版,John Wiley & Sons, Inc,1987年)中之數值。再者,上述文獻中未記載之單體之均聚物之Tg除具有聚有機矽氧烷骨架之單體以外,例如係指可藉由以下之測定方法所獲得之值(參照日本專利特開2007-51271號公報)。即,向具備溫度計、攪拌機、氮氣導入管、及回流冷凝管之反應器中投入單體100質量份、2,2'-偶氮二異丁腈0.2質量份及作為聚合溶劑之乙酸乙酯200質量份,一面導入氮氣一面攪拌1小時。以此方式將聚合系統內之氧去除後,升溫至63℃而反應10小時。其次,冷卻至室溫,獲得固形物成分濃度33質量%之均聚物溶液。其次,將該均聚物溶液流延塗佈於剝離襯墊上,進行乾燥而製作厚度約2 mm之試樣(片狀均聚物)。繼而,將該試樣沖切成直徑7.9 mm之圓盤狀,以平行板將其夾住,使用黏彈性試驗機(商品名「ARES」,Rheometrics公司製造),一面施加頻率1 Hz之剪切應變一面於溫度範圍-70~150℃、5℃/分鐘之升溫速度下藉由剪切模式測定黏彈性,將tanδ之峰頂溫度設為均聚物之Tg。Furthermore, the "glass transition temperature (Tg) when forming a homopolymer" in this specification (sometimes referred to as "Tg of the homopolymer") means "the glass transition temperature (Tg) of the homopolymer of the monomer. )", specifically, the numerical values in "Polymer Handbook" (3rd edition, John Wiley & Sons, Inc, 1987) can be cited. In addition, the Tg of the homopolymer of the monomers not described in the above-mentioned documents, except for the monomers having a polyorganosiloxane skeleton, refers to a value that can be obtained by the following measurement method (refer to Japanese Patent Application Laid-Open). Gazette No. 2007-51271). That is, 100 parts by mass of the monomer, 0.2 parts by mass of 2,2'-azobisisobutyronitrile, and 200 parts by mass of ethyl acetate as the polymerization solvent were put into a reactor equipped with a thermometer, a stirrer, a nitrogen introduction pipe, and a reflux condenser. mass part, and stirred for 1 hour while introducing nitrogen gas. After removing the oxygen in the polymerization system in this way, the temperature was raised to 63°C and the reaction was carried out for 10 hours. Next, it was cooled to room temperature to obtain a homopolymer solution with a solid content concentration of 33% by mass. Next, the homopolymer solution was cast-coated on a release liner and dried to prepare a sample (sheet-shaped homopolymer) with a thickness of approximately 2 mm. Then, the sample was punched into a disc shape with a diameter of 7.9 mm, clamped with parallel plates, and a viscoelasticity testing machine (trade name "ARES", manufactured by Rheometrics Co., Ltd.) was used to apply shear at a frequency of 1 Hz on one side. The strained side was measured in shear mode at a temperature range of -70 to 150°C and a heating rate of 5°C/min. The peak temperature of tan δ was set as the Tg of the homopolymer.
聚合物(A)之重量平均分子量(Mw)較佳為5×10 4以上,更佳為10×10 4以上,進而較佳為20×10 4以上,特佳為30×10 4以上。若上述Mw為5×10 4以上,則易於獲得顯示出良好凝聚性之黏著劑。又,上述Mw較佳為500×10 4以下。若上述Mw為500×10 4以下,則容易形成顯示出適度之流動性(聚合物鏈之運動性)之黏著劑,因此適於實現初始貼附黏著力較低,且加熱後黏著力變高之黏著片材。 The weight average molecular weight (Mw) of the polymer (A) is preferably 5×10 4 or more, more preferably 10×10 4 or more, further preferably 20×10 4 or more, particularly preferably 30×10 4 or more. If the above-mentioned Mw is 5×10 4 or more, an adhesive exhibiting good cohesiveness can be easily obtained. Moreover, the above-mentioned Mw is preferably 500×10 4 or less. If the above-mentioned Mw is 500×10 4 or less, it is easy to form an adhesive showing moderate fluidity (movement of the polymer chain), so it is suitable for achieving low initial adhesion and high adhesion after heating. The adhesive sheet.
再者,於本說明書中,聚合物(A)及聚合物(B)之Mw可藉由凝膠滲透層析法(GPC)進行聚苯乙烯換算來求出。更具體而言,可依據下述實施例中所記載之方法及條件測定Mw。In addition, in this specification, Mw of polymer (A) and polymer (B) can be calculated|required by polystyrene conversion by gel permeation chromatography (GPC). More specifically, Mw can be measured according to the methods and conditions described in the following examples.
上述丙烯酸系聚合物係包含丙烯酸系單體(分子中具有(甲基)丙烯醯基之單體)作為構成聚合物之單體成分的聚合物。即,上述丙烯酸系聚合物包含來自丙烯酸系單體之結構單元。上述丙烯酸系聚合物可僅包含一種丙烯酸系單體作為單體成分,亦可包含兩種以上之丙烯酸系單體作為單體成分。再者,於本說明書中,「(甲基)丙烯酸」表示「丙烯酸」及/或「甲基丙烯酸」(「丙烯酸」及「甲基丙烯酸」中之任一者或兩者),其他亦同。The above-mentioned acrylic polymer is a polymer containing an acrylic monomer (a monomer having a (meth)acrylyl group in the molecule) as a monomer component constituting the polymer. That is, the acrylic polymer contains a structural unit derived from an acrylic monomer. The above-mentioned acrylic polymer may contain only one kind of acrylic monomer as a monomer component, or may contain two or more acrylic monomers as monomer components. Furthermore, in this specification, "(meth)acrylic acid" means "acrylic acid" and/or "methacrylic acid" (either or both of "acrylic acid" and "methacrylic acid"), and the same applies to others. .
上述丙烯酸系聚合物較佳為包含以質量比率計最多之來自(甲基)丙烯酸酯之結構單元的聚合物。作為上述(甲基)丙烯酸酯,例如可例舉含烴基之(甲基)丙烯酸酯。作為上述含烴基之(甲基)丙烯酸酯,可例舉:具有直鏈狀或支鏈狀脂肪族烴基之(甲基)丙烯酸烷基酯、(甲基)丙烯酸環烷基酯等具有脂環式烴基之(甲基)丙烯酸酯、(甲基)丙烯酸芳基酯等具有芳香族烴基之(甲基)丙烯酸酯等。上述含烴基之(甲基)丙烯酸酯可僅使用一種,亦可使用兩種以上。The acrylic polymer is preferably a polymer containing the largest amount of structural units derived from (meth)acrylate in terms of mass ratio. Examples of the (meth)acrylate include hydrocarbon group-containing (meth)acrylate. Examples of the hydrocarbon group-containing (meth)acrylate include (meth)acrylic acid alkyl esters having a linear or branched aliphatic hydrocarbon group, (meth)acrylic acid cycloalkyl esters, and the like having an alicyclic ring. (meth)acrylate having an aromatic hydrocarbon group, such as (meth)acrylate having a hydrocarbon group, aryl (meth)acrylate, etc. Only one type of the above-mentioned hydrocarbon group-containing (meth)acrylate may be used, or two or more types may be used.
作為上述(甲基)丙烯酸烷基酯,例如可例舉:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸異丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸異丁酯、(甲基)丙烯酸第二丁酯、(甲基)丙烯酸第三丁酯、(甲基)丙烯酸戊酯、(甲基)丙烯酸異戊酯、(甲基)丙烯酸己酯、(甲基)丙烯酸庚酯、(甲基)丙烯酸辛酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸異辛酯、(甲基)丙烯酸壬酯、(甲基)丙烯酸異壬酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸異癸酯、(甲基)丙烯酸十一烷基酯、(甲基)丙烯酸十二烷基酯((甲基)丙烯酸月桂酯)、(甲基)丙烯酸十三烷基酯、(甲基)丙烯酸十四烷基酯、(甲基)丙烯酸十五烷基酯、(甲基)丙烯酸十六烷基酯、(甲基)丙烯酸十七烷基酯、(甲基)丙烯酸十八烷基酯、(甲基)丙烯酸十九烷基酯、(甲基)丙烯酸二十烷基酯等。Examples of the alkyl (meth)acrylate include: (methyl)acrylate, ethyl (meth)acrylate, propyl (meth)acrylate, isopropyl (meth)acrylate, (meth)acrylate Butyl methacrylate, isobutyl (meth)acrylate, second butyl (meth)acrylate, third butyl (meth)acrylate, amyl (meth)acrylate, iso(meth)acrylate Pentyl ester, (meth)hexyl acrylate, heptyl (meth)acrylate, octyl (meth)acrylate, 2-ethylhexyl (meth)acrylate, isooctyl (meth)acrylate, (meth)acrylate Nonyl acrylate, isononyl (meth)acrylate, decyl (meth)acrylate, isodecyl (meth)acrylate, undecyl (meth)acrylate, dodecyl (meth)acrylate Alkyl ester (lauryl (meth)acrylate), tridecyl (meth)acrylate, myristyl (meth)acrylate, pentadecyl (meth)acrylate, (meth) Cetyl acrylate, heptadecyl (meth)acrylate, stearyl (meth)acrylate, nonadecyl (meth)acrylate, eicosyl (meth)acrylate wait.
作為上述(甲基)丙烯酸烷基酯,其中,較佳為具有碳數為1~20(較佳為4~12,更佳為6~10)之直鏈狀或支鏈狀脂肪族烴基之(甲基)丙烯酸烷基酯。若上述碳數處於上述範圍內,則上述丙烯酸系聚合物之玻璃轉移溫度之調整較為容易,易於使黏著性更加適宜。The above-mentioned alkyl (meth)acrylate is preferably one having a linear or branched aliphatic hydrocarbon group having a carbon number of 1 to 20 (preferably 4 to 12, more preferably 6 to 10). Alkyl (meth)acrylates. If the carbon number is within the above range, the glass transition temperature of the acrylic polymer can be easily adjusted, and the adhesiveness can be made more suitable.
作為上述(甲基)丙烯酸烷基酯,較佳為至少使用具有碳數為1~18之烷基之(甲基)丙烯酸烷基酯,更佳為使用具有碳數為1~14(較佳為4~12,更佳為6~10)之烷基之丙烯酸烷基酯,特佳為使用丙烯酸正丁酯(BA)及/或丙烯酸2-乙基己酯(2EHA)。As the above-mentioned alkyl (meth)acrylate, it is preferable to use at least an alkyl (meth)acrylate having an alkyl group having a carbon number of 1 to 18, and more preferably an alkyl (meth)acrylate having an alkyl group having a carbon number of 1 to 14. Alkyl acrylate with an alkyl group of 4 to 12, more preferably 6 to 10), particularly preferably n-butyl acrylate (BA) and/or 2-ethylhexyl acrylate (2EHA).
又,作為具有碳數為1~18之烷基之(甲基)丙烯酸烷基酯,可例舉:丙烯酸甲酯、甲基丙烯酸甲酯(MMA)、甲基丙烯酸正丁酯(BMA)、甲基丙烯酸2-乙基己酯(2EHMA)、丙烯酸異硬脂酯(ISTA)等。Moreover, examples of the (meth)acrylic acid alkyl ester having an alkyl group having 1 to 18 carbon atoms include: methyl acrylate, methyl methacrylate (MMA), n-butyl methacrylate (BMA), 2-ethylhexyl methacrylate (2EHMA), isostearyl acrylate (ISTA), etc.
作為上述具有脂環式烴基之(甲基)丙烯酸酯,例如可例舉:(甲基)丙烯酸環戊酯、(甲基)丙烯酸環己酯、(甲基)丙烯酸環庚酯、(甲基)丙烯酸環辛酯等具有一環式脂肪族烴環之(甲基)丙烯酸酯;(甲基)丙烯酸異𦯉基酯等具有二環式脂肪族烴環之(甲基)丙烯酸酯;(甲基)丙烯酸雙環戊酯、(甲基)丙烯酸二環戊氧基乙酯、(甲基)丙烯酸三環戊酯、(甲基)丙烯酸1-金剛烷基酯、(甲基)丙烯酸2-甲基-2-金剛烷基酯、(甲基)丙烯酸2-乙基-2-金剛烷基酯等具有三環以上之脂肪族烴環之(甲基)丙烯酸酯等。Examples of the (meth)acrylate having an alicyclic hydrocarbon group include: (meth)cyclopentyl acrylate, (meth)cyclohexyl acrylate, (meth)cycloheptyl acrylate, (meth)acrylate ) (Meth)acrylates with a monocyclic aliphatic hydrocarbon ring such as cyclooctyl acrylate; (meth)acrylates with a bicyclic aliphatic hydrocarbon ring such as isopropyl (meth)acrylate; (meth)acrylates )Dicyclopentyl acrylate, Dicyclopentyloxyethyl (meth)acrylate, Tricyclopentyl (meth)acrylate, 1-Adamantyl (meth)acrylate, 2-Methyl (meth)acrylate -2-Adamantyl ester, (meth)acrylic acid 2-ethyl-2-adamantyl ester and other (meth)acrylates having three or more aliphatic hydrocarbon rings.
作為上述具有芳香族烴基之(甲基)丙烯酸酯,例如可例舉:(甲基)丙烯酸苯酯、(甲基)丙烯酸苄酯等。Examples of the (meth)acrylate having an aromatic hydrocarbon group include phenyl (meth)acrylate, benzyl (meth)acrylate, and the like.
為了使由上述含烴基之(甲基)丙烯酸酯產生之黏著性等基本特性適當表現於上述黏著劑層中,構成上述丙烯酸系聚合物之全部單體成分中之上述含烴基之(甲基)丙烯酸酯之比率相對於上述全部單體成分之總量(100質量%),較佳為50質量%以上,更佳為60質量%以上,進而較佳為70質量%以上。又,關於上述比率,就可與其他單體成分共聚而獲得該其他單體成分之效果之觀點而言,可為99.9質量%以下,亦可為98質量%以下、95質量%以下、90質量%以下、80質量%以下。In order to appropriately express the basic characteristics such as adhesiveness generated by the above-mentioned hydrocarbon group-containing (meth)acrylate in the above-mentioned adhesive layer, the above-mentioned hydrocarbon group-containing (meth)acrylic acid ester in all monomer components constituting the above-mentioned acrylic polymer The ratio of acrylic acid ester is preferably 50 mass% or more, more preferably 60 mass% or more, and still more preferably 70 mass% or more relative to the total amount (100 mass%) of all the above-mentioned monomer components. In addition, the above ratio may be 99.9 mass% or less, 98 mass% or less, 95 mass% or less, or 90 mass% from the viewpoint that it can be copolymerized with other monomer components to obtain the effects of the other monomer components. % or less, 80 mass% or less.
關於上述丙烯酸系聚合物,為了實現凝聚力之提高或交聯點之導入等改質,亦可包含來自可與上述含烴基之(甲基)丙烯酸酯共聚之其他單體成分的結構單元。作為上述其他單體成分,例如可例舉:含羧基之單體、酸酐單體、含羥基之單體、含縮水甘油基之單體、含磺酸基之單體、含磷酸基之單體、含氮原子之單體等含極性基之單體等。上述其他單體成分可分別僅使用一種,亦可使用兩種以上。The acrylic polymer may contain structural units derived from other monomer components copolymerizable with the hydrocarbon group-containing (meth)acrylate in order to achieve modifications such as improvement of cohesive force or introduction of cross-linking points. Examples of the other monomer components include carboxyl group-containing monomers, acid anhydride monomers, hydroxyl group-containing monomers, glycidyl group-containing monomers, sulfonic acid group-containing monomers, and phosphate group-containing monomers. , monomers containing nitrogen atoms, monomers containing polar groups, etc. Only one type of each of the above-mentioned other monomer components may be used, or two or more types may be used.
作為上述含羧基之單體,例如可例舉:丙烯酸、甲基丙烯酸、(甲基)丙烯酸羧基乙酯、(甲基)丙烯酸羧基戊酯、伊康酸、馬來酸、富馬酸、丁烯酸等。作為上述酸酐單體,例如可例舉:馬來酸酐、伊康酸酐等。Examples of the above carboxyl group-containing monomer include: acrylic acid, methacrylic acid, carboxyethyl (meth)acrylate, carboxypentyl (meth)acrylate, itaconic acid, maleic acid, fumaric acid, butyl Acrylic acid etc. Examples of the acid anhydride monomer include maleic anhydride, itaconic anhydride, and the like.
作為上述含羥基之單體,例如可例舉:(甲基)丙烯酸2-羥基乙酯、(甲基)丙烯酸2-羥基丙酯、(甲基)丙烯酸4-羥基丁酯、(甲基)丙烯酸6-羥基己酯、(甲基)丙烯酸8-羥基辛酯、(甲基)丙烯酸10-羥基癸酯、(甲基)丙烯酸12-羥基月桂酯、(甲基)丙烯酸(4-羥甲基環己基)甲酯等。Examples of the hydroxyl-containing monomer include: (meth)acrylic acid 2-hydroxyethyl ester, (meth)acrylic acid 2-hydroxypropyl ester, (meth)acrylic acid 4-hydroxybutyl ester, (meth)acrylic acid 4-hydroxybutyl ester, (meth)acrylic acid 2-hydroxyethyl 6-hydroxyhexyl acrylate, 8-hydroxyoctyl (meth)acrylate, 10-hydroxydecyl (meth)acrylate, 12-hydroxylauryl (meth)acrylate, (4-hydroxymethyl)acrylate cyclohexyl) methyl ester, etc.
作為上述含縮水甘油基之單體,例如可例舉:(甲基)丙烯酸縮水甘油酯、(甲基)丙烯酸甲基縮水甘油酯等。Examples of the glycidyl group-containing monomer include: glycidyl (meth)acrylate, methylglycidyl (meth)acrylate, and the like.
作為上述含磺酸基之單體,例如可例舉:苯乙烯磺酸、烯丙基磺酸、2-(甲基)丙烯醯胺-2-甲基丙磺酸、(甲基)丙烯醯胺丙磺酸、(甲基)丙烯酸磺丙基酯、(甲基)丙烯醯氧基萘磺酸等。Examples of the above-mentioned sulfonic acid group-containing monomer include: styrenesulfonic acid, allylsulfonic acid, 2-(meth)acrylamide-2-methylpropanesulfonic acid, and (meth)acrylamide. Aminopropyl sulfonic acid, (meth)acrylic acid sulfopropyl ester, (meth)acryloyloxynaphthalene sulfonic acid, etc.
作為上述含磷酸基之單體,例如可例舉2-羥乙基丙烯醯基磷酸酯等。Examples of the phosphoric acid group-containing monomer include 2-hydroxyethylacrylyl phosphate and the like.
上述含氮原子之單體係分子內(1分子內)具有至少1個氮原子之單體(monomer)。上述含氮原子之單體並無特別限定,可較佳地例舉:含環狀氮單體、(甲基)丙烯醯胺類等。再者,含氮原子之單體可僅使用一種,亦可使用兩種以上。The above-mentioned nitrogen atom-containing monomer is a monomer having at least one nitrogen atom in the molecule (within one molecule). The above-mentioned nitrogen atom-containing monomer is not particularly limited, and preferred examples thereof include: cyclic nitrogen-containing monomers, (meth)acrylamides, and the like. Furthermore, only one type of nitrogen atom-containing monomer may be used, or two or more types may be used.
上述含環狀氮單體只要包含(甲基)丙烯醯基或乙烯基等具有不飽和雙鍵之聚合性官能基,且具有環狀氮結構即可,並無特別限定。上述環狀氮結構較佳為於環狀結構內具有氮原子者。The above-mentioned cyclic nitrogen-containing monomer is not particularly limited as long as it contains a polymerizable functional group having an unsaturated double bond such as a (meth)acryl group or a vinyl group and has a cyclic nitrogen structure. The above-mentioned cyclic nitrogen structure preferably has a nitrogen atom in the cyclic structure.
作為上述含環狀氮單體,例如可例舉:N-乙烯基環狀醯胺(內醯胺類乙烯基單體)、具有含氮雜環之乙烯系單體等。Examples of the cyclic nitrogen-containing monomer include N-vinyl cyclic amide (lactam vinyl monomer), vinyl monomers having nitrogen-containing heterocycles, and the like.
作為上述N-乙烯基環狀醯胺,例如可例舉下述式(1)所表示之N-乙烯基環狀醯胺。 [化1] (式(1)中,R 1表示二價有機基) Examples of the N-vinyl cyclic amide include N-vinyl cyclic amide represented by the following formula (1). [Chemical 1] (In formula (1), R 1 represents a divalent organic group)
上述式(1)中之R 1為二價有機基,較佳為二價飽和烴基或不飽和烴基,更佳為二價飽和烴基(例如,碳數3~5之伸烷基等)。 R 1 in the above formula (1) is a divalent organic group, preferably a divalent saturated hydrocarbon group or an unsaturated hydrocarbon group, more preferably a divalent saturated hydrocarbon group (for example, an alkylene group having 3 to 5 carbon atoms, etc.).
作為上述式(1)所表示之N-乙烯基環狀醯胺,例如可例舉:N-乙烯基-2-吡咯啶酮、N-乙烯基-2-哌啶酮、N-乙烯基-3-𠰌啉酮、N-乙烯基-2-己內醯胺、N-乙烯基-1,3-㗁𠯤-2-酮、N-乙烯基-3,5-𠰌啉二酮等。Examples of the N-vinyl cyclic amide represented by the above formula (1) include N-vinyl-2-pyrrolidone, N-vinyl-2-piperidone, N-vinyl- 3-𠰌linone, N-vinyl-2-caprolactam, N-vinyl-1,3-㗁𠯤-2-one, N-vinyl-3,5-𠰌lindione, etc.
作為上述具有含氮雜環之乙烯系單體,例如可例舉:𠰌啉環、哌啶環、吡咯啶環、哌𠯤環等具有含氮雜環之丙烯酸系單體等。Examples of the vinyl monomer having a nitrogen-containing heterocycle include acrylic monomers having a nitrogen-containing heterocycle such as a pyridine ring, a piperidine ring, a pyrrolidine ring, a piperidine ring, and the like.
上述具有含氮雜環之乙烯系單體並無特別限定,例如可例舉:(甲基)丙烯醯𠰌啉、N-乙烯基哌𠯤、N-乙烯基吡咯、N-乙烯基咪唑、N-乙烯基吡𠯤、N-乙烯基𠰌啉、N-乙烯基吡唑、乙烯基吡啶、乙烯基嘧啶、乙烯基㗁唑、乙烯基異㗁唑、乙烯基噻唑、乙烯基異噻唑、乙烯基嗒𠯤、(甲基)丙烯醯基吡咯啶酮、(甲基)丙烯醯基吡咯啶、(甲基)丙烯醯基哌啶等。The above-mentioned vinyl monomer having a nitrogen-containing heterocycle is not particularly limited, and examples thereof include: (meth)acrylamide, N-vinyl piperazole, N-vinylpyrrole, N-vinylimidazole, N -Vinylpyridine, N-vinylpyridine, N-vinylpyrazole, vinylpyridine, vinylpyrimidine, vinylethazole, vinylisethazole, vinylthiazole, vinylisothiazole, vinyl Acrylic acid, (meth)acrylylpyrrolidine, (meth)acrylylpyrrolidine, (meth)acrylylpiperidine, etc.
作為上述(甲基)丙烯醯胺類,例如可例舉:(甲基)丙烯醯胺、N-烷基(甲基)丙烯醯胺、N,N-二烷基(甲基)丙烯醯胺等。作為上述N-烷基(甲基)丙烯醯胺,例如可例舉:N-乙基(甲基)丙烯醯胺、N-異丙基(甲基)丙烯醯胺、N-正丁基(甲基)丙烯醯胺、N-辛基(甲基)丙烯醯胺等。進而,上述N-烷基(甲基)丙烯醯胺亦包括二甲胺基乙基(甲基)丙烯醯胺、二乙胺基乙基(甲基)丙烯醯胺、二甲胺基丙基(甲基)丙烯醯胺之類的具有胺基之(甲基)丙烯醯胺。作為上述N,N-二烷基(甲基)丙烯醯胺,例如可例舉:N,N-二甲基(甲基)丙烯醯胺、N,N-二乙基(甲基)丙烯醯胺、N,N-二丙基(甲基)丙烯醯胺、N,N-二異丙基(甲基)丙烯醯胺、N,N-二(正丁基)(甲基)丙烯醯胺、N,N-二(第三丁基)(甲基)丙烯醯胺等。Examples of the (meth)acrylamides include (meth)acrylamide, N-alkyl(meth)acrylamide, and N,N-dialkyl(meth)acrylamide. wait. Examples of the N-alkyl(meth)acrylamide include N-ethyl(meth)acrylamide, N-isopropyl(meth)acrylamide, N-n-butyl( Meth)acrylamide, N-octyl(meth)acrylamide, etc. Furthermore, the above-mentioned N-alkyl (meth)acrylamide also includes dimethylaminoethyl (meth)acrylamide, diethylaminoethyl (meth)acrylamide, and dimethylaminopropyl (Meth)acrylamide, such as (meth)acrylamide, has an amine group. Examples of the N,N-dialkyl(meth)acrylamide include N,N-dimethyl(meth)acrylamide and N,N-diethyl(meth)acrylamide. Amine, N,N-dipropyl(meth)acrylamide, N,N-diisopropyl(meth)acrylamide, N,N-di(n-butyl)(meth)acrylamide , N,N-di(tert-butyl)(meth)acrylamide, etc.
又,上述(甲基)丙烯醯胺類例如亦包括各種N-羥烷基(甲基)丙烯醯胺。作為上述N-羥烷基(甲基)丙烯醯胺,例如可例舉:N-羥甲基(甲基)丙烯醯胺、N-(2-羥乙基)(甲基)丙烯醯胺、N-(2-羥丙基)(甲基)丙烯醯胺、N-(1-羥丙基)(甲基)丙烯醯胺、N-(3-羥丙基)(甲基)丙烯醯胺、N-(2-羥丁基)(甲基)丙烯醯胺、N-(3-羥丁基)(甲基)丙烯醯胺、N-(4-羥丁基)(甲基)丙烯醯胺、N-甲基-N-2-羥乙基(甲基)丙烯醯胺等。In addition, the above-mentioned (meth)acrylamides also include various N-hydroxyalkyl (meth)acrylamides, for example. Examples of the N-hydroxyalkyl(meth)acrylamide include N-hydroxymethyl(meth)acrylamide, N-(2-hydroxyethyl)(meth)acrylamide, N-(2-hydroxypropyl)(meth)acrylamide, N-(1-hydroxypropyl)(meth)acrylamide, N-(3-hydroxypropyl)(meth)acrylamide , N-(2-hydroxybutyl)(meth)acrylamide, N-(3-hydroxybutyl)(meth)acrylamide, N-(4-hydroxybutyl)(meth)acrylamide Amine, N-methyl-N-2-hydroxyethyl (meth)acrylamide, etc.
又,上述(甲基)丙烯醯胺類例如亦包括各種N-烷氧基烷基(甲基)丙烯醯胺。作為上述N-烷氧基烷基(甲基)丙烯醯胺,例如可例舉:N-甲氧基甲基(甲基)丙烯醯胺、N-丁氧基甲基(甲基)丙烯醯胺等。In addition, the above-mentioned (meth)acrylamides also include various N-alkoxyalkyl (meth)acrylamides, for example. Examples of the N-alkoxyalkyl(meth)acrylamide include N-methoxymethyl(meth)acrylamide and N-butoxymethyl(meth)acrylamide. Amines etc.
又,作為除上述含環狀氮單體、上述(甲基)丙烯醯胺類以外之含氮原子之單體,例如可例舉:含胺基之單體、含氰基之單體、含醯亞胺基之單體、含異氰酸基之單體等。作為上述含胺基之單體,例如可例舉:(甲基)丙烯酸胺基乙酯、(甲基)丙烯酸二甲胺基乙酯、(甲基)丙烯酸二甲胺基丙酯、(甲基)丙烯酸第三丁基胺基乙酯等。作為上述含氰基之單體,例如可例舉:丙烯腈、甲基丙烯腈等。作為上述含醯亞胺基之單體,可例舉:馬來醯亞胺系單體(例如,N-環己基馬來醯亞胺、N-異丙基馬來醯亞胺、N-月桂基馬來醯亞胺、N-苯基馬來醯亞胺等)、伊康醯亞胺系單體(例如,N-甲基伊康醯亞胺、N-乙基伊康醯亞胺、N-丁基伊康醯亞胺、N-辛基伊康醯亞胺、N-2-乙基己基伊康醯亞胺、N-月桂基伊康醯亞胺、N-環己基伊康醯亞胺等)、丁二醯亞胺系單體(例如,N-(甲基)丙烯醯氧基亞甲基丁二醯亞胺、N-(甲基)丙烯醯基-6-氧基六亞甲基丁二醯亞胺、N-(甲基)丙烯醯基-8-氧基八亞甲基丁二醯亞胺等)等。作為上述含異氰酸基之單體,例如可例舉異氰酸2-(甲基)丙烯醯氧基乙酯等。In addition, examples of nitrogen atom-containing monomers other than the above-mentioned cyclic nitrogen-containing monomers and the above-mentioned (meth)acrylamides include: amine group-containing monomers, cyano group-containing monomers, and Imide-based monomers, isocyanate-containing monomers, etc. Examples of the above-mentioned amine group-containing monomer include: (meth)aminoethyl acrylate, (meth)acrylic acid dimethylaminoethyl, (meth)acrylic acid dimethylaminopropyl, (meth)acrylate base) tert-butylaminoethyl acrylate, etc. Examples of the cyano group-containing monomer include acrylonitrile, methacrylonitrile, and the like. Examples of the above-mentioned amide group-containing monomer include maleimide monomers (for example, N-cyclohexylmaleimide, N-isopropylmaleimide, N-laurylimide, etc.). methyl maleimide, N-phenyl maleimide, etc.), itonimide monomers (for example, N-methyl itonimide, N-ethyl itonimide, N-butyliconimide, N-octyliconimide, N-2-ethylhexyliconimide, N-lauryl itonimide, N-cyclohexyliconimide imine, etc.), succinimide-based monomers (for example, N-(meth)acryloxymethylenesuccinimide, N-(meth)acrylyl-6-oxyhexane Methylene succinimide, N-(meth)acryl-8-oxyoctamethylene succinimide, etc.). Examples of the isocyanate group-containing monomer include 2-(meth)acryloyloxyethyl isocyanate.
其中,作為上述含氮原子之單體,較佳為含環狀氮單體,更佳為N-乙烯基環狀醯胺。更具體而言,特佳為N-乙烯基-2-吡咯啶酮(NVP)、N-乙烯基-2-己內醯胺。Among them, as the above-mentioned nitrogen atom-containing monomer, a cyclic nitrogen-containing monomer is preferred, and an N-vinyl cyclic amide is more preferred. More specifically, N-vinyl-2-pyrrolidone (NVP) and N-vinyl-2-caprolactam are particularly preferred.
較佳為含有含羥基之單體及/或含氮原子之單體作為構成上述丙烯酸系聚合物之上述含極性基之單體。藉由使用此種含極性基之單體,可調整黏著劑之凝聚力或極性,而提高加熱後黏著力。It is preferable to contain a hydroxyl group-containing monomer and/or a nitrogen atom-containing monomer as the polar group-containing monomer constituting the acrylic polymer. By using this polar group-containing monomer, the cohesion or polarity of the adhesive can be adjusted, thereby improving the adhesive force after heating.
於上述丙烯酸系聚合物含有上述含羥基之單體作為構成聚合物之單體成分之情形時,構成上述丙烯酸系聚合物之全部單體成分(100質量%)中之上述含羥基之單體之比率並無特別限定,較佳為0.01質量%以上,更佳為0.1質量%以上,進而較佳為0.5質量%以上,進而較佳為1質量%以上,進而較佳為5質量%以上,特佳為10質量%以上。又,關於上述含氮原子之單體之比率,就提高常溫(25℃)下之觸黏感或提高低溫下之柔軟性之觀點而言,較佳為40質量%以下,更佳為30質量%以下,進而較佳為20質量%以下,亦可為10質量%以下或5質量%以下。When the above-mentioned acrylic polymer contains the above-mentioned hydroxyl-containing monomer as a monomer component constituting the polymer, the proportion of the above-mentioned hydroxyl-containing monomer in the total monomer components (100% by mass) constituting the above-mentioned acrylic polymer The ratio is not particularly limited, but it is preferably 0.01% by mass or more, more preferably 0.1% by mass or more, still more preferably 0.5% by mass or more, still more preferably 1% by mass or more, still more preferably 5% by mass or more, especially Preferably, it is 10 mass % or more. In addition, from the viewpoint of improving the tackiness at normal temperature (25°C) or improving the softness at low temperature, the ratio of the above-mentioned nitrogen atom-containing monomer is preferably 40 mass % or less, and more preferably 30 mass %. % or less, more preferably 20 mass% or less, and may be 10 mass% or less or 5 mass% or less.
於上述丙烯酸系聚合物含有上述含氮原子之單體作為構成聚合物之單體成分之情形時,構成上述丙烯酸系聚合物之全部單體成分(100質量%)中之上述含氮原子之單體之比率並無特別限定,較佳為0.01質量%以上,更佳為0.1質量%以上,進而較佳為0.5質量%以上,進而較佳為1質量%以上,進而較佳為5質量%以上,特佳為10質量%以上。又,關於上述含氮原子之單體之比率,就提高常溫(25℃)下之觸黏感或提高低溫下之柔軟性之觀點而言,較佳為40質量%以下,更佳為30質量%以下,進而較佳為20質量%以下。When the acrylic polymer contains the nitrogen-containing monomer as a monomer component constituting the polymer, the nitrogen-containing monomer in all monomer components (100 mass %) constituting the acrylic polymer The ratio of solids is not particularly limited, but is preferably 0.01 mass% or more, more preferably 0.1 mass% or more, further preferably 0.5 mass% or more, further preferably 1 mass% or more, still more preferably 5 mass% or more , the best value is more than 10% by mass. In addition, from the viewpoint of improving the tackiness at normal temperature (25°C) or improving the softness at low temperature, the ratio of the above-mentioned nitrogen atom-containing monomer is preferably 40 mass % or less, and more preferably 30 mass %. % or less, and more preferably 20 mass% or less.
構成上述丙烯酸系聚合物之全部單體成分(100質量%)中之上述含極性基之單體(尤其是上述含氮原子之單體及上述含羥基之單體之合計)之合計比率並無特別限定,就更好地發揮出使用含極性基之單體所獲得之效果之觀點而言,較佳為0.1質量%以上,更佳為1質量%以上,進而較佳為5質量%以上,亦可為10質量%以上、15質量%以上、20質量%以上、或25質量%以上。又,關於上述比率之合計,就獲得具有適度之柔軟性之黏著劑層之觀點而言,較佳為50質量%以下,更佳為40質量%以下。The total ratio of the above-mentioned polar group-containing monomers (especially the total of the above-mentioned nitrogen atom-containing monomers and the above-mentioned hydroxyl group-containing monomers) among all the monomer components (100% by mass) constituting the above-mentioned acrylic polymer has no Specifically limited, from the viewpoint of better exerting the effect obtained by using the polar group-containing monomer, it is preferably 0.1 mass% or more, more preferably 1 mass% or more, and still more preferably 5 mass% or more. It may be 10 mass% or more, 15 mass% or more, 20 mass% or more, or 25 mass% or more. Moreover, from the viewpoint of obtaining an adhesive layer having moderate flexibility, the total of the above ratios is preferably 50 mass% or less, and more preferably 40 mass% or less.
作為構成上述丙烯酸系聚合物之單體成分,可進而包含其他單體。作為上述其他單體,例如可例舉:乙酸乙烯酯、丙酸乙烯酯、月桂酸乙烯酯等乙烯酯系單體;苯乙烯、取代苯乙烯(α-甲基苯乙烯等)、乙烯基甲苯等芳香族乙烯基化合物;乙烯、丙烯、異戊二烯、丁二烯、異丁烯等烯烴系單體;氯乙烯、偏二氯乙烯等含氯單體;(甲基)丙烯酸甲氧基乙酯、(甲基)丙烯酸乙氧基乙酯等含烷氧基之單體;甲基乙烯基醚、乙基乙烯基醚等乙烯醚系單體等。As the monomer component constituting the acrylic polymer, other monomers may be further included. Examples of the other monomers include vinyl ester monomers such as vinyl acetate, vinyl propionate, and vinyl laurate; styrene, substituted styrene (α-methylstyrene, etc.), vinyl toluene and other aromatic vinyl compounds; olefin monomers such as ethylene, propylene, isoprene, butadiene, and isobutylene; chlorine-containing monomers such as vinyl chloride and vinylidene chloride; methoxyethyl (meth)acrylate , ethoxyethyl (meth)acrylate and other alkoxy group-containing monomers; vinyl ether monomers such as methyl vinyl ether and ethyl vinyl ether, etc.
構成上述丙烯酸系聚合物之全部單體成分之總量100質量%中之上述其他單體之比率例如可為0.05質量%以上、0.5質量%以上。上述比率例如可為20質量%以下、10質量%以下、5質量%以下,亦可實質上不含有上述其他單體。The ratio of the other monomers in the total amount of 100% by mass of all monomer components constituting the acrylic polymer may be, for example, 0.05% by mass or more or 0.5% by mass or more. The above-mentioned ratio may be, for example, 20 mass% or less, 10 mass% or less, or 5 mass% or less, or the other monomers described above may not be substantially contained.
上述丙烯酸系聚合物可藉由使上述各種單體成分聚合來獲得。該聚合方法並無特別限定,例如可例舉:溶液聚合方法、乳化聚合方法、塊狀聚合方法、利用活性能量線照射之聚合方法(活性能量線聚合方法)等。又,所獲得之丙烯酸系聚合物可為無規共聚物、嵌段共聚物、接枝共聚物等中之任一者。 The above-mentioned acrylic polymer can be obtained by polymerizing the above-mentioned various monomer components. The polymerization method is not particularly limited, and examples thereof include a solution polymerization method, an emulsion polymerization method, a block polymerization method, a polymerization method using active energy ray irradiation (active energy ray polymerization method), and the like. Moreover, the obtained acrylic polymer may be any of a random copolymer, a block copolymer, a graft copolymer, etc.
於單體成分之聚合時,可使用各種一般之溶劑。作為上述溶劑,例如可例舉:乙酸乙酯、乙酸正丁酯等酯類;甲苯、苯等芳香族烴類;正己烷、正庚烷等脂肪族烴類;環己烷、甲基環己烷等脂環式烴類;甲基乙基酮、甲基異丁基酮等酮類等有機溶劑。上述溶劑可僅使用一種,亦可使用兩種以上。During the polymerization of monomer components, various general solvents can be used. Examples of the solvent include esters such as ethyl acetate and n-butyl acetate; aromatic hydrocarbons such as toluene and benzene; aliphatic hydrocarbons such as n-hexane and n-heptane; cyclohexane and methylcyclohexane; alicyclic hydrocarbons such as alkanes; organic solvents such as ketones such as methyl ethyl ketone and methyl isobutyl ketone. Only one type of solvent may be used, or two or more types of solvents may be used.
單體成分之自由基聚合中所使用之聚合起始劑、鏈轉移劑、乳化劑等並無特別限定,可適當選擇加以使用。再者,丙烯酸系聚合物之重量平均分子量可藉由聚合起始劑、鏈轉移劑之使用量、反應條件來進行控制,可根據其等之種類適當調整其使用量。The polymerization initiator, chain transfer agent, emulsifier, etc. used in the radical polymerization of the monomer components are not particularly limited and can be appropriately selected and used. Furthermore, the weight average molecular weight of the acrylic polymer can be controlled by the usage amounts of polymerization initiators and chain transfer agents and reaction conditions, and the usage amounts can be appropriately adjusted according to their types.
作為單體成分之聚合中所使用之聚合起始劑,可根據聚合反應之種類,使用熱聚合起始劑或光聚合起始劑(光起始劑)等。上述聚合起始劑可僅使用一種,亦可使用兩種以上。As a polymerization initiator used for polymerization of monomer components, a thermal polymerization initiator or a photopolymerization initiator (photoinitiator), etc. can be used depending on the type of polymerization reaction. Only one type of the above-mentioned polymerization initiator may be used, or two or more types may be used.
上述熱聚合起始劑並無特別限定,例如可例舉:偶氮系聚合起始劑、過氧化物系聚合起始劑(例如,過氧化二苯甲醯、過氧化順丁烯二酸第三丁酯、過硫酸鉀等過硫酸鹽;過氧化苯甲醯、過氧化氫等)、苯基取代乙烷等取代乙烷系起始劑、芳香族羰基化合物、氧化還原系聚合起始劑等。其中,較佳為日本專利特開2002-69411號公報所揭示之偶氮系聚合起始劑。作為上述偶氮系聚合起始劑,可例舉:2,2'-偶氮二異丁腈、2,2'-偶氮雙-2-甲基丁腈、2,2'-偶氮雙(2-甲基丙酸)二甲酯、4,4'-偶氮雙-4-氰基戊酸等。熱聚合起始劑之使用量為通常之使用量即可,例如可自相對於單體成分100質量份例如為0.01~5質量份,較佳為0.05~3質量份之範圍內進行選擇。The thermal polymerization initiator is not particularly limited, and examples thereof include azo polymerization initiators, peroxide polymerization initiators (for example, dibenzoyl peroxide, maleic acid peroxide). Persulfates such as tributyl ester, potassium persulfate; benzoyl peroxide, hydrogen peroxide, etc.), substituted ethane-based initiators such as phenyl-substituted ethane, aromatic carbonyl compounds, redox-based polymerization initiators wait. Among them, the azo polymerization initiator disclosed in Japanese Patent Application Laid-Open No. 2002-69411 is preferred. Examples of the azo polymerization initiator include 2,2'-azobisisobutyronitrile, 2,2'-azobis-2-methylbutyronitrile, and 2,2'-azobis. (2-Methylpropionic acid) dimethyl ester, 4,4'-azobis-4-cyanovaleric acid, etc. The thermal polymerization initiator may be used in a normal amount, and may be selected from a range of, for example, 0.01 to 5 parts by mass, preferably 0.05 to 3 parts by mass, based on 100 parts by mass of the monomer component.
上述光聚合起始劑並無特別限定,例如可例舉:安息香醚系光聚合起始劑、苯乙酮系光聚合起始劑、α-酮醇系光聚合起始劑、芳香族磺醯氯系光聚合起始劑、光活性肟系光聚合起始劑、安息香系光聚合起始劑、苯偶醯系光聚合起始劑、二苯甲酮系光聚合起始劑、縮酮系光聚合起始劑、9-氧硫𠮿系光聚合起始劑等。此外,可例舉:醯基氧化膦系光聚合起始劑、二茂鈦系光聚合起始劑。作為上述安息香醚系光聚合起始劑,例如可例舉:安息香甲醚、安息香乙醚、安息香丙醚、安息香異丙醚、安息香異丁醚、2,2-二甲氧基-1,2-二苯乙烷-1-酮、大茴香醚甲醚等。作為上述苯乙酮系光聚合起始劑,例如可例舉:2,2-二乙氧基苯乙酮、2,2-二甲氧基-2-苯基苯乙酮、1-羥基環己基苯基酮、4-苯氧基二氯苯乙酮、4-(第三丁基)二氯苯乙酮等。作為上述α-酮醇系光聚合起始劑,例如可例舉:2-甲基-2-羥基苯丙酮、1-[4-(2-羥乙基)苯基]-2-甲基丙烷-1-酮等。作為上述芳香族磺醯氯系光聚合起始劑,例如可例舉2-萘磺醯氯等。作為上述光活性肟系光聚合起始劑,例如可例舉1-苯基-1,1-丙二酮-2-(O-乙氧羰基)-肟等。作為上述安息香系光聚合起始劑,例如可例舉安息香等。作為上述苯偶醯系光聚合起始劑,例如可例舉苯偶醯等。作為上述二苯甲酮系光聚合起始劑,例如可例舉:二苯甲酮、苯甲醯苯甲酸、3,3'-二甲基-4-甲氧基二苯甲酮、聚乙烯二苯甲酮、α-羥基環己基苯基酮等。作為上述縮酮系光聚合起始劑,例如可例舉苯偶醯二甲基縮酮等。作為上述9-氧硫𠮿系光聚合起始劑,例如可例舉:9-氧硫𠮿、2-氯9-氧硫𠮿、2-甲基9-氧硫𠮿、2,4-二甲基9-氧硫𠮿、異丙基9-氧硫𠮿、2,4-二異丙基9-氧硫𠮿、十二烷基9-氧硫𠮿等。作為上述醯基氧化膦系光聚合起始劑,例如可例舉:2,4,6-三甲基苯甲醯基-二苯基-氧化膦、雙(2,4,6-三甲基苯甲醯基)-苯基氧化膦等。作為上述二茂鈦系光聚合起始劑,例如可例舉雙(η 5-2,4-環戊二烯-1-基)-雙(2,6-二氟-3-(1H-吡咯-1-基)-苯基)鈦等。光聚合起始劑之使用量為通常之使用量即可,例如可自相對於單體成分100質量份例如為0.01~5質量份,較佳為0.05~3質量份之範圍內進行選擇。 The above-mentioned photopolymerization initiator is not particularly limited, and examples thereof include benzoin ether-based photopolymerization initiator, acetophenone-based photopolymerization initiator, α-ketool-based photopolymerization initiator, and aromatic sulfonyl initiator. Chlorine-based photopolymerization initiator, photoactive oxime-based photopolymerization initiator, benzoin-based photopolymerization initiator, benzoyl-based photopolymerization initiator, benzophenone-based photopolymerization initiator, ketal-based photopolymerization initiator Photopolymerization initiator, 9-oxosulfide𠮿 It is a photopolymerization initiator, etc. In addition, examples include phosphine oxide-based photopolymerization initiators and titanocene-based photopolymerization initiators. Examples of the benzoin ether photopolymerization initiator include: benzoin methyl ether, benzoin ethyl ether, benzoin propyl ether, benzoin isopropyl ether, benzoin isobutyl ether, and 2,2-dimethoxy-1,2- Diphenylethane-1-one, anisole methyl ether, etc. Examples of the acetophenone-based photopolymerization initiator include: 2,2-diethoxyacetophenone, 2,2-dimethoxy-2-phenylacetophenone, and 1-hydroxyacetophenone. Hexyl phenyl ketone, 4-phenoxydichloroacetophenone, 4-(tert-butyl)dichloroacetophenone, etc. Examples of the α-ketool photopolymerization initiator include 2-methyl-2-hydroxypropiophenone and 1-[4-(2-hydroxyethyl)phenyl]-2-methylpropane. -1-one etc. Examples of the aromatic sulfonyl chloride-based photopolymerization initiator include 2-naphthalene sulfonyl chloride and the like. Examples of the photoactive oxime-based photopolymerization initiator include 1-phenyl-1,1-propanedione-2-(O-ethoxycarbonyl)-oxime. Examples of the benzoin-based photopolymerization initiator include benzoin and the like. Examples of the benzilyl-based photopolymerization initiator include benzilyl and the like. Examples of the benzophenone-based photopolymerization initiator include benzophenone, benzoyl benzoic acid, 3,3'-dimethyl-4-methoxybenzophenone, and polyethylene. Benzophenone, α-hydroxycyclohexyl phenyl ketone, etc. Examples of the ketal-based photopolymerization initiator include benzyl dimethyl ketal and the like. As the above 9-oxosulfide𠮿 It is a photopolymerization initiator, for example: 9-oxosulfide , 2-chloro-9-oxosulfide𠮿 , 2-Methyl 9-oxosulfide𠮿 , 2,4-dimethyl 9-oxosulfide𠮿 , isopropyl 9-oxosulfide𠮿 , 2,4-diisopropyl 9-oxosulfide𠮿 , dodecyl 9-oxosulfide𠮿 wait. Examples of the above-mentioned phosphine oxide-based photopolymerization initiator include: 2,4,6-trimethylbenzoyl-diphenyl-phosphine oxide, bis(2,4,6-trimethyl Benzyl)-phenylphosphine oxide, etc. Examples of the titanocene-based photopolymerization initiator include bis(eta 5 -2,4-cyclopentadien-1-yl)-bis(2,6-difluoro-3-(1H-pyrrole) -1-yl)-phenyl) titanium, etc. The photopolymerization initiator may be used in a normal amount, and may be selected from a range of, for example, 0.01 to 5 parts by mass, preferably 0.05 to 3 parts by mass, based on 100 parts by mass of the monomer component.
關於上述丙烯酸系聚合物,可對如上所述之單體成分中調配有聚合起始劑之單體組合物照射紫外線(UV)而使單體成分之一部分聚合,以由此獲得之部分聚合物(丙烯酸系聚合物漿液)之形態包含於用以形成黏著劑層之黏著劑組合物中。可將包含上述丙烯酸系聚合物漿液之黏著劑組合物塗佈於金屬基材或剝離襯墊等被塗佈體,照射紫外線而完成聚合。即,上述丙烯酸系聚合物漿液可為丙烯酸系聚合物之前驅物。上述黏著劑層例如可使用包含上述丙烯酸系聚合物漿液、聚合物(B)及酚系抗氧化劑之黏著劑組合物來形成。The above-mentioned acrylic polymer can be obtained by irradiating ultraviolet (UV) rays to a monomer composition in which a polymerization initiator is blended with the monomer components as described above to partially polymerize the monomer components. The form of (acrylic polymer slurry) is included in the adhesive composition for forming the adhesive layer. The adhesive composition containing the above-mentioned acrylic polymer slurry can be coated on a coated object such as a metal substrate or a release liner, and then irradiated with ultraviolet rays to complete polymerization. That is, the acrylic polymer slurry may be an acrylic polymer precursor. The adhesive layer can be formed, for example, using an adhesive composition containing the acrylic polymer slurry, polymer (B), and phenolic antioxidant.
(聚合物(B)) 聚合物(B)包含具有聚有機矽氧烷骨架之單體(B1)及均聚物之玻璃轉移溫度為40℃以上之單體(B2)作為單體單元。 (Polymer (B)) The polymer (B) contains a monomer (B1) having a polyorganosiloxane skeleton and a monomer (B2) having a homopolymer with a glass transition temperature of 40° C. or above as monomer units.
構成聚合物(B)之具有聚有機矽氧烷骨架之單體(B1)並無特別限定,可使用任意之含有聚有機矽氧烷骨架之單體。單體(B1)由於其結構而極性較低,故而積極地促進聚合物(B)於被黏著體表面之不均分佈,表現出貼合初期之易剝離性。The monomer (B1) having a polyorganosiloxane skeleton constituting the polymer (B) is not particularly limited, and any monomer containing a polyorganosiloxane skeleton can be used. Monomer (B1) has low polarity due to its structure, so it actively promotes the uneven distribution of polymer (B) on the surface of the adherend, showing easy peelability in the early stage of lamination.
作為可用作單體(B1)之具有聚有機矽氧烷骨架之單體,例如可例舉:下述式(2)所表示之化合物、下述式(3)所表示之化合物。更具體而言,可例舉:商品名「X-22-174ASX」、商品名「X-22-2475」、商品名「X-22-174DX」、商品名「X-22-2426」、商品名「KF-2012」(以上,信越化學工業股份有限公司製造)等單末端反應性聚矽氧油等。單體(B1)可僅使用一種,亦可使用兩種以上。Examples of the monomer having a polyorganosiloxane skeleton that can be used as the monomer (B1) include a compound represented by the following formula (2) and a compound represented by the following formula (3). More specifically, examples include: product name "X-22-174ASX", product name "X-22-2475", product name "X-22-174DX", product name "X-22-2426", product name Single-terminal reactive polysiloxane oils such as "KF-2012" (above, manufactured by Shin-Etsu Chemical Industry Co., Ltd.). Only one type of monomer (B1) may be used, or two or more types may be used.
[化2] [於式(2)、(3)中,R 2表示氫原子或甲基,R 3表示一價有機基,m及n分別獨立地表示0以上之整數] [Chemicalization 2] [In formulas (2) and (3), R 2 represents a hydrogen atom or a methyl group, R 3 represents a monovalent organic group, and m and n each independently represent an integer above 0]
作為上述一價有機基,可例舉直鏈狀或支鏈狀之烴基。上述烴基為飽和或不飽和烴基。上述一價有機基中之碳數較佳為1~10,更佳為1~4。作為上述一價有機基,其中較佳為:甲基、乙基、丙基(正丙基、異丙基)、丁基(正丁基、第三丁基等)。Examples of the monovalent organic group include linear or branched hydrocarbon groups. The above-mentioned hydrocarbon groups are saturated or unsaturated hydrocarbon groups. The number of carbon atoms in the above-mentioned monovalent organic group is preferably 1 to 10, more preferably 1 to 4. As the above-mentioned monovalent organic group, preferred ones include methyl, ethyl, propyl (n-propyl, isopropyl), and butyl (n-butyl, tert-butyl, etc.).
單體(B1)之官能基當量為1000 g/mol以上且未達15000 g/mol。若官能基當量未達1000 g/mol,則存在無法表現出易剝離性,於貼合初期黏著力不會降低之情況。又,若官能基當量為15000 g/mol以上,則存在與聚合物(A)之相容性顯著變差,與被黏著體貼合初期黏著力不會降低之情況、或黏著力之經時上升性較差之情況。The functional group equivalent of monomer (B1) is 1000 g/mol or more and less than 15000 g/mol. If the functional group equivalent weight is less than 1000 g/mol, it may not be easy to peel off and the adhesive force may not be reduced in the initial stage of lamination. In addition, if the functional group equivalent is 15000 g/mol or more, the compatibility with the polymer (A) may significantly deteriorate, and the adhesive force may not decrease in the initial stage of bonding to the adherend, or the adhesive force may increase over time. Poor sexual performance.
此處,「官能基當量」意指與每個官能基鍵結之主骨架(例如聚二甲基矽氧烷)之質量。關於標記單位g/mol,換算成官能基1 mol。具有聚有機矽氧烷骨架之單體之官能基當量例如可根據利用核磁共振(NMR)分析所獲得之 1H-NMR(質子NMR)之光譜強度進行計算。 Here, "functional group equivalent" means the mass of the main skeleton (eg, polydimethylsiloxane) bonded to each functional group. Regarding the labeling unit g/mol, it is converted into 1 mol of functional group. The functional group equivalent of the monomer having a polyorganosiloxane skeleton can be calculated, for example, based on the spectral intensity of 1 H-NMR (proton NMR) obtained by nuclear magnetic resonance (NMR) analysis.
藉由 1H-NMR,求出經由C鍵結於矽氧烷結構之矽的H(例如Si-(CH 3) 2之H)之光譜強度與官能基之C-CH 3之H、SH之H、或C=CH 2之H之光譜強度之比。以求出矽氧烷結構之Si-(CH 3) 2之H之光譜強度與官能基之C=CH 2之H之光譜強度之比之情況為例進行說明,根據光譜強度比,可知測定試樣所含之矽氧烷結構之Si-(CH 3) 2之個數與官能基之C=CH 2之個數之比。由於矽氧烷結構之化學式及官能基之化學式已預先知曉,因此根據矽氧烷結構之Si-(CH 3) 2之個數與官能基之C=CH 2之個數之比,可知測定試樣中所含之具有Si-(CH 3) 2鍵之矽氧烷結構之個數A與官能基之個數B之比(A/B)。已知每1個具有Si-(CH 3) 2鍵之矽氧烷結構(此處為二甲基矽氧烷)之分子量,因此其每1個之分子量乘以上述矽氧烷結構之個數A與官能基之個數之比(A/B)所得之值即為每個官能基之具有Si-(CH 3) 2鍵之矽氧烷結構之質量,即主骨架之質量,其質量乘以阿佛加德羅常數所得之值即為官能基當量(g/mol)。 By 1 H-NMR, the spectral intensity of H of silicon bonded to the siloxane structure via C (for example, H of Si-(CH 3 ) 2 ) and the H of C-CH 3 and SH of the functional group are determined. The ratio of the spectral intensity of H, or C=CH 2 . Take the case of finding the ratio of the spectral intensity of H of Si-(CH 3 ) 2 of the siloxane structure to the spectral intensity of C=CH 2 of the functional group as an example to illustrate. According to the spectral intensity ratio, it can be seen that the measurement test The ratio of the number of Si-(CH 3 ) 2 in the siloxane structure contained in the sample to the number of C=CH 2 in the functional group. Since the chemical formula of the siloxane structure and the chemical formula of the functional group are known in advance, the measurement test can be determined based on the ratio of the number of Si-(CH 3 ) 2 in the siloxane structure to the number of C=CH 2 in the functional group. The ratio of the number A of siloxane structures with Si-(CH 3 ) 2 bonds to the number B of functional groups contained in the sample (A/B). The molecular weight of each siloxane structure (here, dimethylsiloxane) with Si-(CH 3 ) 2 bonds is known. Therefore, the molecular weight of each siloxane structure is multiplied by the number of the above siloxane structures. The value obtained by the ratio of A to the number of functional groups (A/B) is the mass of the siloxane structure with Si-(CH 3 ) 2 bonds for each functional group, that is, the mass of the main skeleton, and its mass is multiplied by The value obtained from Avogadro's constant is the functional group equivalent (g/mol).
再者,於使用官能基當量不同之兩種以上之具有聚有機矽氧烷骨架之單體之情形時,關於單體(B1)之官能基當量,使用對上述兩種以上之具有聚有機矽氧烷骨架之單體之官能基當量進行算術平均所得之值。例如於使用n種具有聚有機矽氧烷骨架之單體(單體1、單體2、…單體n)之情形時,將利用下式進行計算所得之值設為單體(B1)之官能基當量。 單體(B1)之官能基當量(g/mol)=(單體1之官能基當量×單體1之調配量+單體2之官能基當量×單體2之調配量+…+單體n之官能基當量×單體n之調配量)/(單體1之調配量+單體2之調配量+…+單體n之調配量) Furthermore, when two or more monomers having a polyorganosiloxane skeleton with different functional group equivalents are used, as for the functional group equivalent of the monomer (B1), the above two or more types of polyorganosiloxane skeletons are used. The value obtained by the arithmetic average of the functional group equivalents of the monomers of the oxyalkane skeleton. For example, when n types of monomers (monomer 1, monomer 2, ... monomer n) having a polyorganosiloxane skeleton are used, the value calculated using the following formula is set as monomer (B1) Functional group equivalent. The functional group equivalent of monomer (B1) (g/mol) = (the functional group equivalent of monomer 1 × the blending amount of monomer 1 + the functional group equivalent of monomer 2 × the blending amount of monomer 2 +... + monomer The functional group equivalent of n×the blending amount of monomer n)/(the blending amount of monomer 1+the blending amount of monomer 2+...+the blending amount of monomer n)
關於構成聚合物(B)之全部單體成分中之單體(B1)之比率,就發揮出適度之初始黏著力,且更好地發揮出作為黏著力上升延遲劑之效果之觀點而言,相對於上述全部單體成分之總量(100質量%),較佳為5質量%以上,更佳為10質量%以上,進而較佳為15質量%以上,特佳為20質量%以上。關於上述單體(B1)之比率,就聚合反應性或相容性優異,且黏著力之經時上升性更加優異之觀點而言,相對於上述全部單體成分之總量(100質量%),較佳為60質量%以下,更佳為50質量%以下,進而較佳為40質量%以下,特佳為30質量%以下。Regarding the ratio of the monomer (B1) among the total monomer components constituting the polymer (B), from the viewpoint of exerting a moderate initial adhesive force and better exerting the effect as an adhesive force increase delaying agent, It is preferably 5 mass% or more, more preferably 10 mass% or more, further preferably 15 mass% or more, particularly preferably 20 mass% or more, relative to the total amount (100 mass%) of all the above-mentioned monomer components. Regarding the ratio of the above-mentioned monomer (B1), from the viewpoint of excellent polymerization reactivity or compatibility, and further excellent increase in adhesive force over time, it is based on the total amount of all the above-mentioned monomer components (100% by mass) , preferably 60 mass% or less, more preferably 50 mass% or less, further preferably 40 mass% or less, particularly preferably 30 mass% or less.
關於構成聚合物(B)之單體(B2),均聚物之玻璃轉移溫度為40℃以上,較佳為80℃以上,更佳為100℃以上。單體(B2)可僅使用一種,亦可使用兩種以上。Regarding the monomer (B2) constituting the polymer (B), the glass transition temperature of the homopolymer is 40°C or higher, preferably 80°C or higher, and more preferably 100°C or higher. Only one type of monomer (B2) may be used, or two or more types may be used.
作為單體(B2),可例舉:丙烯酸系單體或含極性基之單體。即,單體(B2)可例舉上述丙烯酸系單體及含極性基之單體中之均聚物之玻璃轉移溫度為40℃以上之單體。Examples of the monomer (B2) include an acrylic monomer or a polar group-containing monomer. That is, examples of the monomer (B2) include monomers in which the glass transition temperature of the homopolymer among the above-mentioned acrylic monomers and polar group-containing monomers is 40° C. or higher.
關於作為丙烯酸系單體之單體(B2),較佳為具有烴基之(甲基)丙烯酸酯,更佳為具有直鏈狀或支鏈狀脂肪族烴基之(甲基)丙烯酸烷基酯、具有脂環式烴基之(甲基)丙烯酸酯。Regarding the monomer (B2) as the acrylic monomer, (meth)acrylate having a hydrocarbon group is preferred, and alkyl (meth)acrylate having a linear or branched aliphatic hydrocarbon group is more preferred. (Meth)acrylate with alicyclic hydrocarbon group.
關於作為丙烯酸系單體之單體(B2),例如可例舉:甲基丙烯酸雙環戊酯(Tg:175℃)、丙烯酸雙環戊酯(Tg:120℃)、甲基丙烯酸異𦯉基酯(Tg:173℃)、丙烯酸異𦯉基酯(Tg:97℃)、甲基丙烯酸甲酯(Tg:105℃)、甲基丙烯酸1-金剛烷基酯(Tg:250℃)、丙烯酸1-金剛烷基酯(Tg:153℃)等。Examples of the monomer (B2) as an acrylic monomer include: dicyclopentyl methacrylate (Tg: 175°C), dicyclopentyl acrylate (Tg: 120°C), isopropyl methacrylate ( Tg: 173℃), isopropyl acrylate (Tg: 97℃), methyl methacrylate (Tg: 105℃), 1-adamantyl methacrylate (Tg: 250℃), 1-adamantyl acrylate Alkyl ester (Tg: 153°C), etc.
關於作為含極性基之單體之單體(B2),可例舉:丙烯醯𠰌啉(Tg:145℃)、二甲基丙烯醯胺(Tg:119℃)、二乙基丙烯醯胺(Tg:81℃)、二甲胺基丙基丙烯醯胺(Tg:134℃)、異丙基丙烯醯胺(Tg:134℃)、羥乙基丙烯醯胺(Tg:98℃)等含醯胺基之單體;N-乙烯基-2-己內醯胺等N-乙烯基己內醯胺等內醯胺類單體等含氮原子之單體等。Examples of the monomer (B2) that is a polar group-containing monomer include acryloline (Tg: 145°C), dimethacrylamide (Tg: 119°C), diethylacrylamide ( Tg: 81℃), dimethylaminopropylacrylamide (Tg: 134℃), isopropylacrylamide (Tg: 134℃), hydroxyethylacrylamide (Tg: 98℃), etc. Amine-based monomers; N-vinyl-2-caprolactam and other lactam monomers such as N-vinyl caprolactam and other nitrogen-containing monomers.
於單體(B2)為含極性基之單體之情形時,聚合物(B)較佳為除單體(B1)及單體(B2)以外,還包含丙烯酸系單體作為構成聚合物(B)之單體成分。When the monomer (B2) is a polar group-containing monomer, the polymer (B) preferably contains, in addition to the monomer (B1) and the monomer (B2), an acrylic monomer as a constituent polymer ( B) monomer components.
關於構成聚合物(B)之全部單體成分中之單體(B2)之比率,就發揮出適度之初始黏著力,且更好地發揮出作為黏著力上升延遲劑之效果之觀點而言,相對於上述全部單體成分之總量(100質量%),較佳為10質量%以上,更佳為20質量%以上,進而較佳為30質量%以上。若上述比率為10質量%以上,則初始黏著力容易降低。關於上述單體(B2)之比率,就聚合反應性或相容性優異,且黏著力之經時上升性更加優異之觀點而言,相對於上述全部單體成分之總量(100質量%),較佳為80質量%以下,更佳為60質量%以下,進而較佳為50質量%以下。Regarding the ratio of the monomer (B2) among all the monomer components constituting the polymer (B), from the viewpoint of exerting a moderate initial adhesive force and better exerting the effect as an adhesive force increase delaying agent, It is preferably 10 mass% or more, more preferably 20 mass% or more, and still more preferably 30 mass% or more relative to the total amount (100 mass%) of all the above-mentioned monomer components. If the above ratio is 10% by mass or more, the initial adhesive force is likely to decrease. Regarding the ratio of the above-mentioned monomer (B2), from the viewpoint of excellent polymerization reactivity or compatibility, and further excellent increase in adhesive force over time, it is based on the total amount of all the above-mentioned monomer components (100% by mass) , preferably 80 mass% or less, more preferably 60 mass% or less, further preferably 50 mass% or less.
作為構成聚合物(B)之單體成分,除單體(B1)及單體(B2)以外,還可包含其他單體。作為上述其他單體,可例舉上文中構成丙烯酸系聚合物之單體之例示及說明中之不屬於單體(B1)及單體(B2)者。上述其他單體較佳為包含均聚物之玻璃轉移溫度未達40℃之單體(有時稱為「單體(B3)」)。單體(B3)之均聚物之玻璃轉移溫度未達40℃,較佳為35℃以下,更佳為30℃以下。單體(B3)可僅使用一種,亦可使用兩種以上。As the monomer component constituting the polymer (B), other monomers may be included in addition to the monomer (B1) and the monomer (B2). Examples of the above-mentioned other monomers include those other than the monomer (B1) and the monomer (B2) in the above examples and descriptions of the monomers constituting the acrylic polymer. The above-mentioned other monomers are preferably monomers including homopolymers with a glass transition temperature of less than 40° C. (sometimes referred to as “monomer (B3)”). The glass transition temperature of the homopolymer of monomer (B3) is less than 40°C, preferably 35°C or less, more preferably 30°C or less. Only one type of monomer (B3) may be used, or two or more types may be used.
作為單體(B3),可例舉丙烯酸系單體。即,單體(B3)可例舉上述丙烯酸系單體中之均聚物之玻璃轉移溫度未達40℃之單體。關於作為丙烯酸系單體之單體(B3),例如可例舉:甲基丙烯酸丁酯(Tg:20℃)、甲基丙烯酸2-乙基己酯(Tg:-10℃)等甲基丙烯酸烷基酯等。Examples of the monomer (B3) include acrylic monomers. That is, the monomer (B3) may be a monomer in which the glass transition temperature of the homopolymer among the above-mentioned acrylic monomers is less than 40°C. Examples of the acrylic monomer (B3) include methacrylic acid such as butyl methacrylate (Tg: 20°C) and 2-ethylhexyl methacrylate (Tg: -10°C). Alkyl esters, etc.
構成聚合物(B)之全部單體成分中之單體(B3)之比率相對於上述全部單體成分之總量(100質量%),較佳為10質量%以上,更佳為20質量%以上,進而較佳為30質量%以上。上述比率相對於上述全部單體成分之總量(100質量%),較佳為85質量%以下,更佳為70質量%以下,進而較佳為55質量%以下,特佳為50質量%以下。The ratio of the monomer (B3) among all the monomer components constituting the polymer (B) is preferably 10 mass% or more, more preferably 20 mass% relative to the total amount of all the above-mentioned monomer components (100 mass%) or more, and more preferably 30% by mass or more. The above ratio is preferably 85 mass% or less, more preferably 70 mass% or less, further preferably 55 mass% or less, particularly preferably 50 mass% or less, based on the total amount (100 mass%) of all the above-mentioned monomer components. .
構成聚合物(B)之全部單體成分中之單體(B1)及單體(B2)之合計比率相對於上述全部單體成分之總量(100質量%),較佳為15質量%以上,更佳為30質量%以上,進而較佳為45質量%以上,特佳為50質量%以上。上述合計比率相對於上述全部單體成分之總量(100質量%),較佳為90質量%以下,更佳為80質量%以下,進而較佳為70質量%以下。The total ratio of the monomer (B1) and the monomer (B2) among all the monomer components constituting the polymer (B) is preferably 15 mass% or more relative to the total amount of all the above-mentioned monomer components (100 mass%) , more preferably 30 mass% or more, still more preferably 45 mass% or more, and particularly preferably 50 mass% or more. The above total ratio is preferably 90 mass% or less, more preferably 80 mass% or less, and still more preferably 70 mass% or less relative to the total amount (100 mass%) of all the above-mentioned monomer components.
聚合物(B)之重量平均分子量為10000以上且未達100000,較佳為12000以上且未達50000,更佳為15000以上且未達30000。若聚合物(B)之重量平均分子量為100000以上,則貼合初期之接著力便不會降低。又,若重量平均分子量未達10000,則分子量較低,因而存在黏著片材之黏著力不會隨時間上升之情況。The weight average molecular weight of the polymer (B) is 10,000 or more and less than 100,000, preferably 12,000 or more and less than 50,000, more preferably 15,000 or more and less than 30,000. If the weight average molecular weight of the polymer (B) is 100,000 or more, the adhesive strength in the initial stage of bonding will not be reduced. In addition, if the weight average molecular weight is less than 10,000, the molecular weight is low, so the adhesive force of the adhesive sheet may not increase with time.
聚合物(B)例如可藉由使上述各種單體成分聚合而獲得。該聚合方法並無特別限定,可例舉:溶液聚合方法、乳化聚合方法、塊狀聚合方法、利用活性能量線照射之聚合方法(活性能量線聚合方法)等。 The polymer (B) can be obtained, for example, by polymerizing the various monomer components described above. The polymerization method is not particularly limited, and examples include a solution polymerization method, an emulsion polymerization method, a block polymerization method, a polymerization method using active energy ray irradiation (active energy ray polymerization method), and the like.
於上述聚合中,可使用鏈轉移劑以調整聚合物(B)之分子量。作為上述鏈轉移劑,可例舉:辛硫醇、月桂硫醇、第三壬硫醇、第三-十二硫醇、巰基乙醇、α-硫代甘油等具有巰基之化合物;硫代乙醇酸、硫代乙醇酸甲酯、硫代乙醇酸乙酯、硫代乙醇酸丙酯、硫代乙醇酸丁酯、硫代乙醇酸第三丁酯、硫代乙醇酸2-乙基己酯、硫代乙醇酸辛酯、硫代乙醇酸異辛酯、硫代乙醇酸癸酯、硫代乙醇酸十二烷基酯、乙二醇之硫代乙醇酸酯、新戊二醇之硫代乙醇酸酯、季戊四醇之硫代乙醇酸酯等硫代乙醇酸酯類;α-甲基苯乙烯二聚物等。上述鏈轉移劑可僅使用一種,亦可使用兩種以上。In the above polymerization, a chain transfer agent can be used to adjust the molecular weight of polymer (B). Examples of the chain transfer agent include compounds having mercapto groups such as octyl mercaptan, lauryl mercaptan, tertiary nonyl mercaptan, tertiary dodecyl mercaptan, mercaptoethanol, α-thioglycerol and the like; thioglycolic acid , methyl thioglycolate, ethyl thioglycolate, propyl thioglycolate, butyl thioglycolate, tert-butyl thioglycolate, 2-ethylhexyl thioglycolate, sulfide Octyl glycolate, isooctyl thioglycolate, decyl thioglycolate, dodecyl thioglycolate, thioglycolate of ethylene glycol, thioglycolate of neopentyl glycol , thioglycolic acid esters such as pentaerythritol thioglycolic acid ester; α-methylstyrene dimer, etc. Only one type of the above-mentioned chain transfer agent may be used, or two or more types may be used.
上述鏈轉移劑之使用量相對於單體成分100質量份,例如為0.05~20質量份,較佳為0.1~15質量份,更佳為0.2~10質量份。The usage amount of the above chain transfer agent is, for example, 0.05 to 20 parts by mass, preferably 0.1 to 15 parts by mass, and more preferably 0.2 to 10 parts by mass relative to 100 parts by mass of the monomer component.
上述黏著劑層中之聚合物(B)之含量相對於聚合物(A)之總量100質量份,為0.1~20質量份,較佳為0.3~25質量份,更佳為0.4~20質量份,進而較佳為0.5~15質量份,進而更佳為1~10質量份,特佳為2~7質量份。藉由使上述含量為0.1質量份以上,而二次加工性優異。藉由使上述含量為20質量份以下,可於加熱後實現較高之黏著力。The content of the polymer (B) in the adhesive layer is 0.1 to 20 parts by mass, preferably 0.3 to 25 parts by mass, and more preferably 0.4 to 20 parts by mass relative to 100 parts by mass of the total amount of polymer (A). parts, more preferably 0.5 to 15 parts by mass, still more preferably 1 to 10 parts by mass, particularly preferably 2 to 7 parts by mass. By setting the above content to 0.1 parts by mass or more, secondary processability is excellent. By making the above content 20 parts by mass or less, higher adhesive force can be achieved after heating.
上述黏著劑層於不損害本發明之效果之範圍內,可包含除聚合物(A)及聚合物(B)以外之其他聚合物。上述其他聚合物之含有比率相對於上述黏著劑層所含之聚合物成分之總量100質量%,較佳為20質量%以下,更佳為15質量%以下,進而較佳為10質量%以下,亦可為5質量%以下、3質量%以下、或1質量%以下。上述黏著劑層較佳為實質上不含有上述其他聚合物之黏著劑層。The above-mentioned adhesive layer may contain polymers other than polymer (A) and polymer (B) within the scope that does not impair the effects of the present invention. The content ratio of the other polymers is preferably 20 mass% or less, more preferably 15 mass% or less, and still more preferably 10 mass% or less based on 100 mass% of the total amount of polymer components contained in the adhesive layer. , it may be 5 mass% or less, 3 mass% or less, or 1 mass% or less. The above-mentioned adhesive layer is preferably an adhesive layer that does not substantially contain the above-mentioned other polymers.
(酚系抗氧化劑) 上述黏著劑層除聚合物(A)及聚合物(B)以外,還包含酚系抗氧化劑。推測上述酚系抗氧化劑具有於上述黏著劑層中捕捉可能成為釋氣之成分之功能,藉由含有特定量以上之酚系抗氧化劑,而黏著劑層之總釋氣量減少。上述酚系抗氧化劑可僅使用一種,亦可使用兩種以上。 (phenolic antioxidant) The above-mentioned adhesive layer contains a phenolic antioxidant in addition to the polymer (A) and the polymer (B). It is speculated that the above-mentioned phenolic antioxidant has the function of capturing components that may become outgassing in the above-mentioned adhesive layer, and by containing a specific amount or more of the phenolic antioxidant, the total amount of outgassing of the adhesive layer is reduced. Only one type of the above-mentioned phenolic antioxidant may be used, or two or more types may be used.
上述酚系抗氧化劑中之酚骨架之數量並無特別限定,為1個以上(例如1~10),較佳為2個以上,更佳為3個以上,進而較佳為4個以上。若上述酚骨架之數量較多,則總釋氣量進而減少。The number of phenolic skeletons in the above-mentioned phenolic antioxidant is not particularly limited. It is 1 or more (for example, 1 to 10), preferably 2 or more, more preferably 3 or more, and still more preferably 4 or more. If the number of the above-mentioned phenolic skeletons is larger, the total gas release amount will further decrease.
作為上述酚系抗氧化劑之具體例,可例舉:2,6-二-第三丁基-對甲酚、2,6-二-第三丁基-4-乙基苯酚、2,6-二環己基-4-甲基苯酚、2,6-二異丙基-4-乙基苯酚、2,6-二第三戊基-4-甲基苯酚、2,6-二第三辛基-4-正丙基苯酚、2,6-二環己基-4-正辛基苯酚、2-異丙基-4-甲基-6-第三丁基苯酚、2-第三丁基-4-乙基-6-第三辛基苯酚、2-異丁基-4-乙基-6-第三己基苯酚、2-環己基-4-正丁基-6-異丙基苯酚、苯乙烯化混合甲酚、DL-α-生育酚、β-(3,5-二-第三丁基-4-羥基苯基)丙酸硬脂酯、2,6-二-第三丁基-4-(4,6-雙(辛硫基)-1,3,5-三𠯤-2-基-胺基)苯酚等具有1個酚骨架之化合物(單環酚化合物);2,2'-亞甲基雙(4-甲基-6-第三丁基苯酚)、4,4'-亞丁基雙(3-甲基-6-第三丁基苯酚)、4,4'-硫代雙(3-甲基-6-第三丁基苯酚)、2,2'-硫代雙(4-甲基-6-第三丁基苯酚)、4,4'-亞甲基雙(2,6-二第三丁基苯酚)、2,2'-亞甲基雙[6-(1-甲基環己基)-對甲酚]、2,2'-亞乙基雙(4,6-二第三丁基苯酚)、2,2'-亞丁基雙(2-第三丁基-4-甲基苯酚)、3,6-二氧雜八亞甲基雙[3-(3-第三丁基-4-羥基-5-甲基苯基)丙酸酯]、三乙二醇雙[3-(3-第三丁基-5-甲基-4-羥基苯基)丙酸酯]、1,6-己二醇雙[3-(3,5-二-第三丁基-4-羥基苯基)丙酸酯]、2,2'-硫代二伸乙基雙[3-(3,5-二-第三丁基-4-羥基苯基)丙酸酯]等具有2個酚骨架之化合物(2環酚化合物);1,1,3-三(2-甲基-4-羥基-5-第三丁基苯基)丁烷、1,3,5-三(2,6-二甲基-3-羥基-4-第三丁基苄基)異氰尿酸酯、1,3,5-三[(3,5-二-第三丁基-4-羥基苯基)丙醯氧基乙基]異氰尿酸酯、三(4-第三丁基-2,6-二甲基-3-羥基苄基)異氰尿酸酯、1,3,5-三甲基-2,4,6-三(3,5-二-第三丁基-4-羥基苄基)苯等具有3個酚骨架之化合物(3環酚化合物);四[亞甲基-3-(3,5-二-第三丁基-4-羥基苯基)丙酸酯]甲烷等具有4個酚骨架之化合物(4環酚化合物);雙(3,5-二-第三丁基-4-羥基苄基膦酸乙酯)鈣、雙(3,5-二-第三丁基-4-羥基苄基膦酸乙酯)鎳等含磷之酚化合物等。Specific examples of the phenolic antioxidant include: 2,6-di-tert-butyl-p-cresol, 2,6-di-tert-butyl-4-ethylphenol, 2,6-di-tert-butyl-p-cresol, Dicyclohexyl-4-methylphenol, 2,6-diisopropyl-4-ethylphenol, 2,6-di-3-pentyl-4-methylphenol, 2,6-di-3-octyl -4-n-propylphenol, 2,6-dicyclohexyl-4-n-octylphenol, 2-isopropyl-4-methyl-6-tert-butylphenol, 2-tert-butyl-4 -Ethyl-6-tert-octylphenol, 2-isobutyl-4-ethyl-6-tert-hexylphenol, 2-cyclohexyl-4-n-butyl-6-isopropylphenol, styrene Chemical mixed cresol, DL-α-tocopherol, β-(3,5-di-tert-butyl-4-hydroxyphenyl)stearyl propionate, 2,6-di-tert-butyl-4 -(4,6-Bis(octylthio)-1,3,5-tri𠯤-2-yl-amino)phenol and other compounds with one phenolic skeleton (monocyclic phenolic compounds); 2,2'- Methylene bis(4-methyl-6-tert-butylphenol), 4,4'-butylene bis(3-methyl-6-tert-butylphenol), 4,4'-thiobis (3-methyl-6-tert-butylphenol), 2,2'-thiobis(4-methyl-6-tert-butylphenol), 4,4'-methylenebis(2, 6-di-tert-butylphenol), 2,2'-methylenebis[6-(1-methylcyclohexyl)-p-cresol], 2,2'-ethylenebis(4,6- Di-tert-butylphenol), 2,2'-butylenebis(2-tert-butyl-4-methylphenol), 3,6-dioxaoctamethylenebis[3-(3-th Tributyl-4-hydroxy-5-methylphenyl)propionate], triethylene glycol bis[3-(3-tert-butyl-5-methyl-4-hydroxyphenyl)propionate ], 1,6-hexanediol bis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate], 2,2'-thiodiethylene bis[3 -(3,5-Di-tert-butyl-4-hydroxyphenyl)propionate] and other compounds with two phenolic skeletons (2-ring phenol compounds); 1,1,3-tris(2-methyl) -4-Hydroxy-5-tert-butylphenyl)butane, 1,3,5-tris(2,6-dimethyl-3-hydroxy-4-tert-butylbenzyl)isocyanuric acid Ester, 1,3,5-tris[(3,5-di-tert-butyl-4-hydroxyphenyl)propyloxyethyl]isocyanurate, tris(4-tert-butyl- 2,6-Dimethyl-3-hydroxybenzyl)isocyanurate, 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4 -Hydroxybenzyl)benzene and other compounds with 3 phenolic skeletons (3-ring phenol compounds); tetrakis[methylene-3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate ]Methane and other compounds with 4 phenolic skeletons (4-ring phenol compounds); bis(3,5-di-tert-butyl-4-hydroxybenzylphosphonate ethyl ester) calcium, bis(3,5-di- Phosphorus-containing phenolic compounds such as ethyl tert-butyl-4-hydroxybenzylphosphonate) nickel, etc.
上述黏著劑層中之上述酚系抗氧化劑之含量相對於聚合物(A)之總量100質量份,為0.4質量份以上,較佳為0.5質量份以上,更佳為0.7質量份以上。藉由使上述含量為0.4質量份以上,而黏著片材之總釋氣量減少。上述含量較佳為未達5質量份,更佳為4質量份以下,進而較佳為3質量份以下。若上述含量未達5質量份,則不易於黏著劑層表面發生偏析,從而不易引起黏著劑層表面之固形化、或受其影響所造成之加熱後之黏著力之降低。又,在形成黏著劑層之黏著劑組合物中之分散性優異。The content of the phenolic antioxidant in the adhesive layer is 0.4 parts by mass or more, preferably 0.5 parts by mass or more, and more preferably 0.7 parts by mass or more based on 100 parts by mass of the total amount of polymer (A). By making the above content 0.4 parts by mass or more, the total outgassing amount of the adhesive sheet is reduced. The above content is preferably less than 5 parts by mass, more preferably 4 parts by mass or less, and still more preferably 3 parts by mass or less. If the above content is less than 5 parts by mass, segregation on the surface of the adhesive layer is less likely to occur, thereby causing solidification of the surface of the adhesive layer or a reduction in the adhesive force after heating due to its influence. Furthermore, it has excellent dispersibility in the adhesive composition forming the adhesive layer.
聚合物(A)與聚合物(B)可藉由交聯劑進行交聯。藉由使用交聯劑,可於黏著劑層中之聚合物成分中形成交聯結構,而控制凝聚力。上述交聯劑可根據聚合物(A)或聚合物(B)等聚合物成分於側鏈上所具有之官能基進行適當選擇。上述交聯劑可僅使用一種,亦可使用兩種以上。Polymer (A) and polymer (B) can be cross-linked by a cross-linking agent. By using a cross-linking agent, a cross-linked structure can be formed in the polymer component in the adhesive layer to control cohesion. The cross-linking agent can be appropriately selected according to the functional groups that polymer components such as polymer (A) or polymer (B) have on their side chains. Only one type of cross-linking agent may be used, or two or more types of cross-linking agents may be used.
上述交聯劑並無特別限定,例如可例舉:異氰酸酯系交聯劑、環氧系交聯劑、三聚氰胺系交聯劑、過氧化物系交聯劑、脲系交聯劑、金屬烷氧化物系交聯劑、金屬螯合物系交聯劑、金屬鹽系交聯劑、碳二醯亞胺系交聯劑、㗁唑啉系交聯劑、氮丙啶系交聯劑、胺系交聯劑、肼系交聯劑、矽酮系交聯劑、矽烷系交聯劑(矽烷偶合劑)等。作為上述交聯劑,其中,較佳為包含異氰酸酯系交聯劑。The above-mentioned cross-linking agent is not particularly limited, and examples thereof include isocyanate-based cross-linking agents, epoxy-based cross-linking agents, melamine-based cross-linking agents, peroxide-based cross-linking agents, urea-based cross-linking agents, and metal alkoxides. Physical cross-linking agent, metal chelate cross-linking agent, metal salt cross-linking agent, carbodiimide cross-linking agent, oxazoline cross-linking agent, aziridine cross-linking agent, amine cross-linking agent Cross-linking agent, hydrazine-based cross-linking agent, silicone-based cross-linking agent, silane-based cross-linking agent (silane coupling agent), etc. The cross-linking agent preferably contains an isocyanate-based cross-linking agent.
上述交聯劑之含量並無特別限定,相對於聚合物(A)之總量100質量份,較佳為0.01質量份以上,更佳為0.05質量份以上,進而較佳為0.1質量份以上,進而更佳為0.5質量份以上,特佳為1質量份以上。若上述含量為0.01質量份以上,則二次加工性更加優異。又,上述交聯劑之含量較佳為15質量份以下,更佳為10質量份以下,進而較佳為5質量份以下。The content of the cross-linking agent is not particularly limited, but is preferably 0.01 parts by mass or more, more preferably 0.05 parts by mass or more, and still more preferably 0.1 parts by mass or more, based on 100 parts by mass of the total amount of polymer (A). More preferably, it is 0.5 parts by mass or more, and particularly preferably, it is 1 part by mass or more. If the content is 0.01 parts by mass or more, the secondary processability will be further excellent. In addition, the content of the cross-linking agent is preferably 15 parts by mass or less, more preferably 10 parts by mass or less, and still more preferably 5 parts by mass or less.
上述異氰酸酯系交聯劑係每1分子具有平均2個以上之異氰酸基之化合物(多官能異氰酸酯化合物)。作為上述異氰酸酯系交聯劑,可例舉:脂肪族聚異氰酸酯類、脂環族聚異氰酸酯類、芳香族聚異氰酸酯類等。The isocyanate cross-linking agent is a compound (polyfunctional isocyanate compound) having an average of two or more isocyanate groups per molecule. Examples of the isocyanate-based crosslinking agent include aliphatic polyisocyanates, alicyclic polyisocyanates, aromatic polyisocyanates, and the like.
作為上述脂肪族聚異氰酸酯類,例如可例舉:1,2-伸乙基二異氰酸酯;1,2-四亞甲基二異氰酸酯、1,3-四亞甲基二異氰酸酯、1,4-四亞甲基二異氰酸酯等四亞甲基二異氰酸酯;1,2-六亞甲基二異氰酸酯、1,3-六亞甲基二異氰酸酯、1,4-六亞甲基二異氰酸酯、1,5-六亞甲基二異氰酸酯、1,6-六亞甲基二異氰酸酯、2,5-六亞甲基二異氰酸酯等六亞甲基二異氰酸酯;2-甲基-1,5-戊烷二異氰酸酯、3-甲基-1,5-戊烷二異氰酸酯;離胺酸二異氰酸酯等。Examples of the aliphatic polyisocyanates include: 1,2-ethylidene diisocyanate; 1,2-tetramethylene diisocyanate, 1,3-tetramethylene diisocyanate, 1,4-tetrakis Tetramethylene diisocyanate such as methylene diisocyanate; 1,2-hexamethylene diisocyanate, 1,3-hexamethylene diisocyanate, 1,4-hexamethylene diisocyanate, 1,5- Hexamethylene diisocyanate, 1,6-hexamethylene diisocyanate, 2,5-hexamethylene diisocyanate and other hexamethylene diisocyanates; 2-methyl-1,5-pentane diisocyanate, 3-methyl-1,5-pentane diisocyanate; lysine diisocyanate, etc.
作為上述脂環族聚異氰酸酯類,例如可例舉:異佛爾酮二異氰酸酯;1,2-環己基二異氰酸酯、1,3-環己基二異氰酸酯、1,4-環己基二異氰酸酯等環己基二異氰酸酯;1,2-環戊基二異氰酸酯、1,3-環戊基二異氰酸酯等環戊基二異氰酸酯;氫化苯二甲基二異氰酸酯、氫化甲苯二異氰酸酯、氫化二苯基甲烷二異氰酸酯、氫化四甲基二甲苯二異氰酸酯、4,4'-二環己基甲烷二異氰酸酯等。Examples of the alicyclic polyisocyanates include isophorone diisocyanate; cyclohexyl diisocyanate such as 1,2-cyclohexyl diisocyanate, 1,3-cyclohexyl diisocyanate, and 1,4-cyclohexyl diisocyanate. Diisocyanates; cyclopentyl diisocyanates such as 1,2-cyclopentyl diisocyanate and 1,3-cyclopentyl diisocyanate; hydrogenated xylylene diisocyanate, hydrogenated toluene diisocyanate, hydrogenated diphenylmethane diisocyanate, Hydrogenated tetramethylxylene diisocyanate, 4,4'-dicyclohexylmethane diisocyanate, etc.
作為上述芳香族聚異氰酸酯類,例如可例舉:2,4-甲苯二異氰酸酯、2,6-甲苯二異氰酸酯、4,4'-二苯基甲烷二異氰酸酯、2,4'-二苯基甲烷二異氰酸酯、2,2'-二苯基甲烷二異氰酸酯、4,4'-二苯醚二異氰酸酯、2-硝基二苯基-4,4'-二異氰酸酯、2,2'-二苯基丙烷-4,4'-二異氰酸酯、3,3'-二甲基二苯基甲烷-4,4'-二異氰酸酯、4,4'-二苯基丙烷二異氰酸酯、間苯二異氰酸酯、對苯二異氰酸酯、伸萘基-1,4-二異氰酸酯、伸萘基-1,5-二異氰酸酯、3,3'-二甲氧基二苯基-4,4'-二異氰酸酯、苯二甲基-1,4-二異氰酸酯、苯二甲基-1,3-二異氰酸酯等。Examples of the aromatic polyisocyanates include 2,4-toluene diisocyanate, 2,6-toluene diisocyanate, 4,4'-diphenylmethane diisocyanate, and 2,4'-diphenylmethane. Diisocyanate, 2,2'-diphenylmethane diisocyanate, 4,4'-diphenyl ether diisocyanate, 2-nitrodiphenyl-4,4'-diisocyanate, 2,2'-diphenyl Propane-4,4'-diisocyanate, 3,3'-dimethyldiphenylmethane-4,4'-diisocyanate, 4,4'-diphenylpropane diisocyanate, isophthalic diisocyanate, p-phenylene Diisocyanate, naphthylene-1,4-diisocyanate, naphthylene-1,5-diisocyanate, 3,3'-dimethoxydiphenyl-4,4'-diisocyanate, xylylenedimethyl -1,4-diisocyanate, xylylenedimethyl-1,3-diisocyanate, etc.
又,作為上述異氰酸酯系交聯劑,例如亦可例舉:三羥甲基丙烷/甲苯二異氰酸酯加成物(商品名「Coronate L」,東曹股份有限公司製造)、三羥甲基丙烷/六亞甲基二異氰酸酯加成物(商品名「Coronate HL」,東曹股份有限公司製造)、三羥甲基丙烷/苯二甲基二異氰酸酯加成物(商品名「Takenate D-110N」,三井化學股份有限公司製造)等市售品。Examples of the isocyanate cross-linking agent include: trimethylolpropane/toluene diisocyanate adduct (trade name "Coronate L", manufactured by Tosoh Co., Ltd.), trimethylolpropane/ Hexamethylene diisocyanate adduct (trade name "Coronate HL", manufactured by Tosoh Co., Ltd.), trimethylolpropane/xylylene diisocyanate adduct (trade name "Takenate D-110N", (manufactured by Mitsui Chemicals Co., Ltd.) and other commercially available products.
作為上述環氧系交聯劑(多官能環氧化合物),例如可例舉:N,N,N',N'-四縮水甘油基-間苯二甲胺、二縮水甘油基苯胺、1,3-雙(N,N-二縮水甘油胺甲基)環己烷、1,6-己二醇二縮水甘油醚、新戊二醇二縮水甘油醚、乙二醇二縮水甘油醚、丙二醇二縮水甘油醚、聚乙二醇二縮水甘油醚、聚丙二醇二縮水甘油醚、山梨醇聚縮水甘油醚、甘油聚縮水甘油醚、季戊四醇聚縮水甘油醚、聚甘油聚縮水甘油醚、山梨醇酐聚縮水甘油醚、三羥甲基丙烷聚縮水甘油醚、己二酸二縮水甘油酯、鄰苯二甲酸二縮水甘油酯、三縮水甘油基-三(2-羥乙基)異氰尿酸酯、間苯二酚二縮水甘油醚、雙酚-S-二縮水甘油醚,除此以外,還可例舉分子內具有2個以上之環氧基之環氧系樹脂等。又,作為上述環氧系交聯劑,例如亦可例舉商品名「Tetrad C」(三菱瓦斯化學股份有限公司製造)等市售品。Examples of the above-mentioned epoxy cross-linking agent (polyfunctional epoxy compound) include: N,N,N',N'-tetraglycidyl-m-xylylenediamine, diglycidylaniline, 1, 3-Bis(N,N-diglycidylaminemethyl)cyclohexane, 1,6-hexanediol diglycidyl ether, neopentyl glycol diglycidyl ether, ethylene glycol diglycidyl ether, propylene glycol diglycidyl ether Glycidyl ether, polyethylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether, sorbitol polyglycidyl ether, glycerol polyglycidyl ether, pentaerythritol polyglycidyl ether, polyglycerol polyglycidyl ether, sorbitan polyglycidyl ether Glycidyl ether, trimethylolpropane polyglycidyl ether, diglycidyl adipate, diglycidyl phthalate, triglycidyl-tris(2-hydroxyethyl)isocyanurate, In addition to resorcinol diglycidyl ether and bisphenol-S-diglycidyl ether, epoxy resins having two or more epoxy groups in the molecule may be used. Examples of the epoxy cross-linking agent include commercially available products such as the trade name "Tetrad C" (manufactured by Mitsubishi Gas Chemical Co., Ltd.).
作為上述過氧化物系交聯劑,只要是藉由熱量產生自由基活性種而促進基礎聚合物之交聯者便可適當使用,考慮到作業性或穩定性,較佳為使用1分鐘半衰期溫度為80~160℃之過氧化物,更佳為使用1分鐘半衰期溫度為90~140℃之過氧化物。As the above-mentioned peroxide cross-linking agent, any one that generates radical active species by heat and promotes the cross-linking of the base polymer can be used appropriately. In consideration of workability and stability, it is preferable to use a half-life temperature of 1 minute. The peroxide is a peroxide of 80 to 160°C, and more preferably a peroxide with a half-life temperature of 90 to 140°C in 1 minute is used.
作為上述過氧化物系交聯劑,例如可例舉:過氧化二碳酸二(2-乙基己基)酯(1分鐘半衰期溫度:90.6℃)、過氧化二碳酸二(4-第三丁基環己基)酯(1分鐘半衰期溫度:92.1℃)、過氧化二碳酸二第二丁酯(1分鐘半衰期溫度:92.4℃)、過氧化新癸酸第三丁酯(1分鐘半衰期溫度:103.5℃)、過氧化特戊酸第三己酯(1分鐘半衰期溫度:109.1℃)、過氧化特戊酸第三丁酯(1分鐘半衰期溫度:110.3℃)、過氧化二月桂醯(1分鐘半衰期溫度:116.4℃)、過氧化二正辛醯(1分鐘半衰期溫度:117.4℃)、過氧化2-乙基己酸1,1,3,3-四甲基丁酯(1分鐘半衰期溫度:124.3℃)、過氧化二(4-甲基苯甲醯)(1分鐘半衰期溫度:128.2℃)、過氧化二苯甲醯(1分鐘半衰期溫度:130.0℃)、過氧化異丁酸第三丁酯(1分鐘半衰期溫度:136.1℃)、1,1-二(第三己基過氧基)環己烷(1分鐘半衰期溫度:149.2℃)等。Examples of the peroxide-based cross-linking agent include di(2-ethylhexyl) peroxydicarbonate (1-minute half-life temperature: 90.6°C), di(4-tert-butyl peroxydicarbonate) Cyclohexyl) ester (half-life temperature in 1 minute: 92.1°C), dibutyl peroxydicarbonate (half-life temperature in 1 minute: 92.4°C), tert-butyl peroxyneodecanoate (half-life temperature in 1 minute: 103.5°C) ), tert-hexyl pivalate peroxide (half-life temperature in 1 minute: 109.1°C), tert-butyl pivalate peroxide (half-life temperature in 1 minute: 110.3°C), dilauryl peroxide (half-life temperature in 1 minute) : 116.4℃), di-n-octyl peroxide (half-life temperature in 1 minute: 117.4℃), 1,1,3,3-tetramethylbutyl peroxide 2-ethylhexanoate (half-life temperature in 1 minute: 124.3℃) ), dibenzoyl peroxide (1-minute half-life temperature: 128.2°C), dibenzoyl peroxide (1-minute half-life temperature: 130.0°C), tert-butyl peroxide isobutyrate ( 1-minute half-life temperature: 136.1°C), 1,1-di(tertiary hexylperoxy)cyclohexane (1-minute half-life temperature: 149.2°C), etc.
上述過氧化物系交聯劑之半衰期係指表示過氧化物之分解速度之指標,係指過氧化物之殘存量成為一半為止之時間。關於用以於任意時間點獲得半衰期之分解溫度、或任意溫度下之半衰期時間,在製造商目錄等中有所記載,例如,日油股份有限公司之「有機過氧化物目錄第9版(2003年5月)」等中有所記載。再者,作為反應處理後所殘存之過氧化物分解量之測定方法,例如可利用HPLC(高效液相層析儀)進行測定。更具體而言,例如,各取出約0.2 g之反應處理後之黏著劑,浸漬於乙酸乙酯10 ml中,利用振盪機於25℃下、120 rpm下振盪提取3小時後,於室溫下靜置3天。其次,添加乙腈10 ml,於25℃下、120 rpm下振盪30分鐘,利用膜濾器(0.45 μm)進行過濾而獲得提取液,將該提取液約10 μl注入HPLC中進行分析,將其設為反應處理後之過氧化物量。The half-life of the above-mentioned peroxide cross-linking agent is an index indicating the decomposition rate of the peroxide, and refers to the time until the remaining amount of the peroxide becomes half. The decomposition temperature used to obtain the half-life at any point in time, or the half-life time at any temperature, is described in manufacturers' catalogs, etc., for example, "Organic Peroxide Catalog 9th Edition (2003) of NOF Co., Ltd. May 2016)" etc. In addition, as a method for measuring the decomposition amount of peroxide remaining after the reaction treatment, HPLC (high performance liquid chromatography) can be used for measurement, for example. More specifically, for example, take out about 0.2 g of the reaction-treated adhesive in each case, immerse it in 10 ml of ethyl acetate, use a shaker to extract at 25°C and 120 rpm for 3 hours, and then place it at room temperature. Let sit for 3 days. Next, 10 ml of acetonitrile was added, shaken at 25°C and 120 rpm for 30 minutes, filtered with a membrane filter (0.45 μm) to obtain an extract, and about 10 μl of the extract was injected into HPLC for analysis, and was set to The amount of peroxide after reaction treatment.
又,作為上述交聯劑,可併用有機系交聯劑或多官能性金屬螯合物。多官能性金屬螯合物係多價金屬與有機化合物進行共價鍵結或配位鍵結而成者。作為多價金屬原子,可例舉:Al、Cr、Zr、Co、Cu、Fe、Ni、V、Zn、In、Ca、Mg、Mn、Y、Ce、Sr、Ba、Mo、La、Sn、Ti等。作為進行共價鍵結或配位鍵結之有機化合物中之原子,可例舉氧原子等,作為有機化合物,可例舉:烷基酯、醇化合物、羧酸化合物、醚化合物、酮化合物等。Furthermore, as the cross-linking agent, an organic cross-linking agent or a polyfunctional metal chelate compound may be used together. Multifunctional metal chelates are formed by covalent bonding or coordination bonding between multivalent metals and organic compounds. Examples of polyvalent metal atoms include: Al, Cr, Zr, Co, Cu, Fe, Ni, V, Zn, In, Ca, Mg, Mn, Y, Ce, Sr, Ba, Mo, La, Sn, Ti et al. Examples of the atom in the organic compound that undergoes covalent bonding or coordination bonding include oxygen atoms. Examples of the organic compound include alkyl esters, alcohol compounds, carboxylic acid compounds, ether compounds, ketone compounds, etc. .
上述黏著劑層於不損害本發明之效果之範圍內,還可包含除上述各成分以外之其他成分。作為上述其他成分,可例舉:硬化劑、交聯觸媒、黏著賦予樹脂、抗老化劑、填充劑(金屬粉、有機填充劑、無機填充劑等)、除酚系抗氧化劑以外之抗氧化劑、塑化劑、軟化劑、界面活性劑、抗靜電劑、表面潤滑劑、調平劑、光穩定劑、紫外線吸收劑、聚合抑制劑、粒狀物、箔狀物、著色劑(顏料、染料等)等。上述其他成分可分別僅使用一種,亦可使用兩種以上。再者,相對於上述黏著劑層中之抗氧化劑之總量100質量%,酚系抗氧化劑之比率較佳為60質量%以上,亦可為70質量%以上、80質量%以上、90質量%以上、95質量%以上、99質量%以上。The above-mentioned adhesive layer may also contain other components in addition to the above-mentioned components within the scope that does not impair the effects of the present invention. Examples of the above-mentioned other components include hardeners, cross-linking catalysts, adhesion-imparting resins, anti-aging agents, fillers (metal powder, organic fillers, inorganic fillers, etc.), and antioxidants other than phenolic antioxidants. , plasticizers, softeners, surfactants, antistatic agents, surface lubricants, leveling agents, light stabilizers, UV absorbers, polymerization inhibitors, granules, foils, colorants (pigments, dyes etc. Only one type of each of the above-mentioned other components may be used, or two or more types may be used. Furthermore, relative to the total amount of antioxidants in the adhesive layer (100 mass%), the ratio of phenolic antioxidants is preferably 60 mass% or more, and may also be 70 mass% or more, 80 mass% or more, or 90 mass%. Above, 95 mass% or above, 99 mass% or above.
上述黏著劑層可含有交聯觸媒。若包含交聯觸媒,則可促進利用交聯劑等進行之交聯反應。作為上述交聯觸媒,較佳為錫系觸媒(尤其是二月桂酸二辛基錫)。上述交聯觸媒可僅使用一種,亦可使用兩種以上。上述交聯觸媒之含量相對於聚合物(A)100質量份,例如為0.0001~1質量份。The above-mentioned adhesive layer may contain a cross-linking catalyst. If a cross-linking catalyst is included, the cross-linking reaction using a cross-linking agent or the like can be accelerated. As the cross-linking catalyst, a tin-based catalyst (especially dioctyltin dilaurate) is preferred. Only one type of the above-mentioned cross-linking catalyst may be used, or two or more types may be used. The content of the cross-linking catalyst is, for example, 0.0001 to 1 part by mass relative to 100 parts by mass of the polymer (A).
上述黏著劑層可含有黏著賦予樹脂。若包含黏著賦予樹脂,則上述黏著劑層即便較薄,仍將具有更加良好之密接性。作為上述黏著賦予樹脂,例如可例舉:酚系黏著賦予樹脂、萜烯系黏著賦予樹脂、松香系黏著賦予樹脂、烴系黏著賦予樹脂、環氧系黏著賦予樹脂、聚醯胺系黏著賦予樹脂、彈性體系黏著賦予樹脂、酮系黏著賦予樹脂等。又,作為上述黏著賦予樹脂,此外還可例舉甲基丙烯酸雙環戊酯(DCPMA)與甲基丙烯酸甲酯(MMA)之低聚物等(甲基)丙烯酸烷基酯之低聚物等。上述黏著賦予樹脂可僅使用一種,亦可使用兩種以上。The adhesive layer may contain an adhesive imparting resin. If an adhesion-imparting resin is included, the adhesive layer will have better adhesion even if it is thin. Examples of the tackifier-imparting resin include phenol-based tackifier-imparting resin, terpene-based tackifier-imparting resin, rosin-based tackifier-imparting resin, hydrocarbon-based tackifier-imparting resin, epoxy-based tackifier-imparting resin, and polyamide-based tackifier-imparting resin. , elastic system adhesion-imparting resin, ketone-based adhesion-imparting resin, etc. Examples of the tackifier-imparting resin include oligomers of (meth)acrylic acid alkyl esters such as oligomers of dicyclopentyl methacrylate (DCPMA) and methyl methacrylate (MMA). Only one type of the above-mentioned tackifying resin may be used, or two or more types may be used.
作為上述酚系黏著賦予樹脂,可例舉:萜酚樹脂、氫化萜酚樹脂、烷基酚樹脂、松香酚醛樹脂。上述萜酚樹脂係包含萜烯殘基及酚殘基之聚合物,可例舉:萜烯類與酚化合物之共聚物(萜烯-酚共聚物樹脂)、萜烯類均聚物或共聚物經酚改性而成者(酚改性萜烯樹脂)。作為構成上述萜酚樹脂之萜烯類,可例舉:α-蒎烯、β-蒎烯、檸檬烯(d體、l體、d/l體(雙戊烯)等)等單萜類。上述氫化萜酚樹脂係具有上述萜酚樹脂經氫化而成之結構之樹脂。上述烷基酚樹脂係由烷基酚及甲醛所獲得之樹脂(油性酚樹脂)。作為上述烷基酚樹脂,例如可例舉:酚醛清漆型及可溶酚醛型者。上述松香酚醛樹脂係松香類或下述各種松香衍生物之酚改性物。作為上述松香酚醛樹脂,例如可藉由以酸觸媒使酚加成至松香類或下述各種松香衍生物並進行熱聚合之方法等來獲得。Examples of the phenolic tackifier-imparting resin include terpene phenol resin, hydrogenated terpene phenol resin, alkyl phenol resin, and rosin phenolic resin. The above-mentioned terpene phenol resin is a polymer containing a terpene residue and a phenol residue. Examples thereof include: copolymers of terpenes and phenol compounds (terpene-phenol copolymer resin), terpene homopolymers or copolymers It is modified by phenol (phenol modified terpene resin). Examples of the terpenes constituting the terpene phenol resin include monoterpenes such as α-pinene, β-pinene, and limonene (d form, l form, d/l form (dipentene), etc.). The hydrogenated terpene phenol resin is a resin having a structure obtained by hydrogenating the above terpene phenol resin. The above-mentioned alkylphenol resin is a resin obtained from alkylphenol and formaldehyde (oil-based phenol resin). Examples of the alkylphenol resin include novolak type and resol type. The above-mentioned rosin phenolic resin is a phenol-modified product of rosin or various rosin derivatives described below. The rosin phenolic resin can be obtained, for example, by adding phenol to rosins or various rosin derivatives described below using an acid catalyst and thermally polymerizing the resin.
作為上述萜烯系黏著賦予樹脂,可例舉:α-蒎烯、β-蒎烯、d-檸檬烯、l-檸檬烯、雙戊烯等萜烯類(典型的是單萜類)之聚合物。上述萜烯類之聚合物可為一種萜烯類之均聚物,亦可為兩種以上之萜烯類之共聚物。作為一種萜烯類之均聚物,可例舉:α-蒎烯聚合物、β-蒎烯聚合物、雙戊烯聚合物等。上述改性萜烯系黏著賦予樹脂係對上述萜烯樹脂進行改性而成者(改性萜烯樹脂)。作為上述改性萜烯樹脂,可例舉:苯乙烯改性萜烯樹脂、氫化萜烯樹脂等。Examples of the terpene-based adhesive-imparting resin include polymers of terpenes (typically monoterpenes) such as α-pinene, β-pinene, d-limonene, l-limonene, and dipentene. The above-mentioned terpene polymer may be a homopolymer of one terpene, or a copolymer of two or more terpenes. Examples of terpene homopolymers include α-pinene polymer, β-pinene polymer, and dipentene polymer. The above-mentioned modified terpene-based adhesive imparting resin is obtained by modifying the above-mentioned terpene resin (modified terpene resin). Examples of the modified terpene resin include styrene-modified terpene resin, hydrogenated terpene resin, and the like.
作為上述松香系黏著賦予樹脂,可例舉:松香類及松香衍生物樹脂。作為上述松香類,例如可例舉:松脂膠、木松香、妥爾油松香等未改性松香(生松香);該等未改性松香藉由氫化、歧化、聚合等進行改性而成之改性松香(氫化松香、歧化松香、聚合松香、經其他化學修飾過之松香等)等。作為上述松香衍生物樹脂,可例舉上述松香類之衍生物。作為上述松香衍生物樹脂,例如可例舉:未改性松香與醇類之酯即未改性松香酯、或改性松香與醇類之酯即改性松香酯等松香酯類;以不飽和脂肪酸對松香類進行改性而成之不飽和脂肪酸改性松香類;以不飽和脂肪酸對松香酯類進行改性而成之不飽和脂肪酸改性松香酯類;松香類或上述各種松香衍生物之羧基進行還原處理而成之松香醇類;松香類或上述各種松香衍生物之金屬鹽等。作為上述松香酯類之具體例,可例舉:未改性松香或改性松香之甲酯、三乙二醇酯、甘油酯、季戊四醇酯等。Examples of the rosin-based tackifier-imparting resin include rosin-based and rosin derivative resins. Examples of the above-mentioned rosins include unmodified rosin (raw rosin) such as rosin gum, wood rosin, and tall oil rosin; these unmodified rosins are modified by hydrogenation, disproportionation, polymerization, etc. Modified rosin (hydrogenated rosin, disproportionated rosin, polymerized rosin, other chemically modified rosin, etc.), etc. Examples of the rosin derivative resin include the above-mentioned rosin derivatives. Examples of the rosin derivative resin include unmodified rosin esters, which are esters of unmodified rosin and alcohols, or modified rosin esters, which are esters of modified rosin and alcohols. Unsaturated fatty acid-modified rosin obtained by modifying rosin with fatty acid; unsaturated fatty acid-modified rosin ester obtained by modifying rosin ester with unsaturated fatty acid; rosin or any of the above-mentioned various rosin derivatives Rosin alcohols obtained by reduction treatment of carboxyl groups; rosins or metal salts of various rosin derivatives mentioned above, etc. Specific examples of the rosin esters include methyl ester of unmodified rosin or modified rosin, triethylene glycol ester, glycerol ester, pentaerythritol ester, and the like.
作為上述烴系黏著賦予樹脂,可例舉:脂肪族烴系樹脂、芳香族烴系樹脂、脂肪族環狀烴系樹脂、脂肪族-芳香族系石油樹脂(苯乙烯-烯烴系共聚物等)、脂肪族-脂環族系石油樹脂、氫化烴系樹脂、苯并呋喃系樹脂、苯并呋喃-茚系樹脂等。Examples of the hydrocarbon-based tackifier-imparting resin include aliphatic hydrocarbon-based resins, aromatic hydrocarbon-based resins, aliphatic cyclic hydrocarbon-based resins, aliphatic-aromatic petroleum resins (styrene-olefin-based copolymers, etc.) , aliphatic-alicyclic petroleum resin, hydrogenated hydrocarbon resin, benzofuran resin, benzofuran-indene resin, etc.
上述黏著劑層可為任意形態,例如可為乳液型、溶劑型(溶液型)、活性能量線硬化型、熱熔型(hot melt型)等。其中,就易於獲得生產性優異之黏著劑層之方面而言,較佳為溶劑型、活性能量線硬化型黏著劑組合物。The above-mentioned adhesive layer can be in any form, for example, it can be emulsion type, solvent type (solution type), active energy ray curing type, hot melt type (hot melt type), etc. Among them, in terms of easily obtaining an adhesive layer with excellent productivity, a solvent-based or active energy ray-curable adhesive composition is preferred.
上述黏著劑層之厚度(單面之黏著劑層之總厚度)並無特別限定,例如為1 μm以上,較佳為3 μm以上,更佳為5 μm以上,進而較佳為8 μm以上。上述厚度例如為30 μm以下,較佳為15 μm以下。若上述厚度為30 μm以下,則可使黏著片材之總釋氣量降低。再者,於上述黏著片材為雙面黏著片材之情形時,雙面之黏著劑層之厚度可相同,亦可不同。The thickness of the above-mentioned adhesive layer (the total thickness of the adhesive layer on one side) is not particularly limited. For example, it is 1 μm or more, preferably 3 μm or more, more preferably 5 μm or more, and still more preferably 8 μm or more. The thickness is, for example, 30 μm or less, preferably 15 μm or less. If the above thickness is 30 μm or less, the total gas release amount of the adhesive sheet can be reduced. Furthermore, when the above-mentioned adhesive sheet is a double-sided adhesive sheet, the thickness of the adhesive layer on both sides may be the same or different.
上述黏著劑層可為任意形態,例如可為乳液型、溶劑型(溶液型)、活性能量線硬化型、熱熔型(hot melt型)等。其中,就易於獲得生產性優異之黏著劑層之方面而言,較佳為溶劑型、活性能量線硬化型黏著劑組合物。The above-mentioned adhesive layer can be in any form, for example, it can be emulsion type, solvent type (solution type), active energy ray curing type, hot melt type (hot melt type), etc. Among them, in terms of easily obtaining an adhesive layer with excellent productivity, a solvent-based or active energy ray-curable adhesive composition is preferred.
作為上述活性能量線,例如可例舉:α射線、β射線、γ射線、中子射線、電子束等游離輻射、或紫外線等,特佳為紫外線。即,上述活性能量線硬化型黏著劑層較佳為紫外線硬化型黏著劑層。Examples of the active energy rays include ionizing radiation such as alpha rays, beta rays, gamma rays, neutron rays, and electron beams, or ultraviolet rays. Ultraviolet rays are particularly preferred. That is, the active energy ray curable adhesive layer is preferably an ultraviolet curable adhesive layer.
上述黏著劑層例如可將用以形成黏著劑層之黏著劑組合物塗佈(塗敷)於金屬基材或剝離襯墊等被塗佈體,使所獲得之黏著劑組合物層乾燥硬化來製造;或者將上述黏著劑組合物塗佈(塗敷)於被塗佈體,對所獲得之黏著劑組合物層照射活性能量線使其硬化來製造。又,亦可視需要進而進行加熱乾燥。上述黏著劑組合物較佳為包含聚合物(A)、聚合物(B)、及酚系抗氧化劑。The above-mentioned adhesive layer can be formed by coating (coating) the adhesive composition used to form the adhesive layer on a coated object such as a metal substrate or a release liner, and drying and hardening the obtained adhesive composition layer. Manufacturing; or manufacturing by coating (coating) the above-mentioned adhesive composition on the object to be coated, and irradiating the obtained adhesive composition layer with active energy rays to harden it. In addition, heating and drying may be further performed if necessary. The above-mentioned adhesive composition preferably contains polymer (A), polymer (B), and phenolic antioxidant.
(黏著片材) 上述黏著片材之厚度較佳為10~350 μm,更佳為13~100 μm。進而較佳為15~60 μm以上。若上述厚度為10 μm以上,則操作性優異。若上述厚度為350 μm以下,則可使黏著片材之厚度更薄。再者,上述黏著片材之厚度係指一黏著面至另一黏著面之厚度即黏著體之厚度,並不包含剝離襯墊。 (adhesive sheet) The thickness of the above-mentioned adhesive sheet is preferably 10 to 350 μm, more preferably 13 to 100 μm. Furthermore, it is more preferable that it is 15-60 micrometer or more. If the thickness is 10 μm or more, the workability will be excellent. If the above thickness is 350 μm or less, the thickness of the adhesive sheet can be made even thinner. Furthermore, the thickness of the above-mentioned adhesive sheet refers to the thickness from one adhesive surface to the other adhesive surface, that is, the thickness of the adhesive body, and does not include the release liner.
上述黏著片材之總釋氣量較佳為15500 ppm以下,更佳為13000 ppm以下,進而較佳為10000 ppm以下,特佳為3000 ppm以下。上述總釋氣量越少,就環境保護之觀點而言越佳。上述總釋氣量可藉由頂空進樣器於200℃下將5 cm 2尺寸之黏著片材加熱60分鐘,將加熱後之氣相部分1 mL注入氣相層析儀中進行測定。更詳細而言,可於實施例所記載之條件下進行測定。 The total outgassing amount of the adhesive sheet is preferably 15,500 ppm or less, more preferably 13,000 ppm or less, further preferably 10,000 ppm or less, particularly preferably 3,000 ppm or less. The smaller the above-mentioned total gas release amount, the better it is from the viewpoint of environmental protection. The above total gas release amount can be measured by heating a 5 cm 2 size adhesive sheet at 200°C for 60 minutes with a headspace sampler, and injecting 1 mL of the heated gas phase into a gas chromatograph. More specifically, the measurement can be performed under the conditions described in the examples.
上述黏著片材之金屬基材表面之表面電阻值較佳為10 -1Ω/cm 2以下,更佳為10 -2Ω/cm 2以下,進而較佳為10 -3Ω/cm 2以下,特佳為10 -4Ω/cm 2以下。上述表面電阻值可於溫度23℃、50%RH之氣體氛圍下,基於JIS K6911,使用URS探針,於外加電壓10 V、外加時間10秒之條件下進行測定。 The surface resistance value of the metal substrate surface of the above-mentioned adhesive sheet is preferably 10 -1 Ω/cm 2 or less, more preferably 10 -2 Ω/cm 2 or less, and further preferably 10 -3 Ω/cm 2 or less. Particularly preferred is 10 -4 Ω/cm 2 or less. The above surface resistance value can be measured in a gas atmosphere with a temperature of 23°C and 50% RH, based on JIS K6911, using a URS probe, with an applied voltage of 10 V and an applied time of 10 seconds.
將上述黏著片材貼合於SUS304BA板並於23℃之環境下放置30分鐘後之180°剝離黏著力(初始黏著力)較佳為4 N/25 mm以下,更佳為2 N/25 mm以下,進而較佳為0.5 N/25 mm以下,特佳為0.3 N/25 mm以下。若上述初始黏著力為4 N/25 mm以下,則二次加工性優異。關於上述初始黏著力,就貼合於被黏著體時不易剝落之觀點而言,較佳為0.05 N/25 mm以上。The above adhesive sheet is attached to the SUS304BA board and placed in an environment of 23°C for 30 minutes. The 180° peeling adhesive force (initial adhesive force) is preferably 4 N/25 mm or less, and more preferably 2 N/25 mm. or less, more preferably 0.5 N/25 mm or less, particularly preferably 0.3 N/25 mm or less. If the above-mentioned initial adhesion force is 4 N/25 mm or less, the secondary processability will be excellent. The above-mentioned initial adhesive force is preferably 0.05 N/25 mm or more from the viewpoint of not easily peeling off when attached to the adherend.
將上述黏著片材貼合於SUS304BA板並於80℃之環境下放置5分鐘後之180°剝離黏著力(加熱後黏著力)較佳為10 N/25 mm以上,更佳為15 N/25 mm以上,進而較佳為18 N/25 mm以上,特佳為20 N/25 mm以上。The above adhesive sheet is attached to the SUS304BA board and placed in an environment of 80°C for 5 minutes. The 180° peeling adhesive force (adhesive force after heating) is preferably 10 N/25 mm or more, and more preferably 15 N/25 mm or more, more preferably 18 N/25 mm or more, particularly preferably 20 N/25 mm or more.
上述黏著片材可在使用前於黏著劑層之表面(黏著面)貼合有剝離襯墊。於上述黏著片材為雙面黏著片材之情形時,上述黏著片材中之雙面之各黏著面可分別藉由2片剝離襯墊加以保護,亦可藉由1片雙面成為剝離面之剝離襯墊,以捲繞成卷狀之形態(捲繞體)加以保護。剝離襯墊用作黏著劑層之保護材,於貼附於被黏著體時被剝離。再者,並非必須設置剝離襯墊。The above-mentioned adhesive sheet can be pasted with a release liner on the surface (adhesive surface) of the adhesive layer before use. When the above-mentioned adhesive sheet is a double-sided adhesive sheet, each of the two-sided adhesive surfaces in the above-mentioned adhesive sheet can be protected by two pieces of release liners, or one double-sided piece can be used as the release surface. The release liner is rolled into a roll for protection. The release liner is used as a protective material for the adhesive layer and is peeled off when it is attached to the adherend. Furthermore, it is not necessary to provide a release liner.
作為上述剝離襯墊,可使用習用之剝離紙等,並無特別限定,例如可例舉:具有剝離處理層之基材、包含氟聚合物之低接著性基材或包含無極性聚合物之低接著性基材等。作為上述具有剝離處理層之基材,例如可例舉:經矽酮系、長鏈烷基系、氟系、硫化鉬等剝離處理劑表面處理之塑膠膜或紙等。作為上述包含氟聚合物之低接著性基材中之氟系聚合物,例如可例舉:聚四氟乙烯、聚氯三氟乙烯、聚氟乙烯、聚偏二氟乙烯、四氟乙烯-六氟丙烯共聚物、氯氟乙烯-偏二氟乙烯共聚物等。又,作為上述無極性聚合物,例如可例舉:烯烴系樹脂(例如,聚乙烯、聚丙烯等)等。再者,剝離襯墊可藉由公知或習用之方法來形成。又,剝離襯墊之厚度亦無特別限定。As the above-mentioned release liner, conventional release paper, etc. can be used without particular limitation. Examples thereof include: a base material having a release treatment layer, a low-adhesion base material containing a fluoropolymer, or a low-adhesion base material containing a non-polar polymer. Adhesive substrates, etc. Examples of the base material having a release treatment layer include plastic film or paper surface-treated with release treatment agents such as silicone-based, long-chain alkyl-based, fluorine-based, and molybdenum sulfide. Examples of the fluorine-based polymer in the low-adhesion base material containing a fluoropolymer include polytetrafluoroethylene, polychlorotrifluoroethylene, polyvinyl fluoride, polyvinylidene fluoride, and tetrafluoroethylene-hexafluoroethylene. Fluoropropylene copolymer, chlorofluoroethylene-vinylidene fluoride copolymer, etc. Examples of the nonpolar polymer include olefin resins (for example, polyethylene, polypropylene, etc.). Furthermore, the release liner can be formed by a known or conventional method. In addition, the thickness of the release liner is not particularly limited.
上述黏著片材可用於貼合被黏著體之公知或習用之用途。其中,上述黏著片材較佳為用於使黏著劑層貼合於絕緣層之絕緣層貼附用途。又,關於上述黏著片材,就總釋氣量較少且導電性優異之觀點而言,較佳為電池構件貼附用途,更佳為全固體電池構件貼附用途。作為電池構件貼附用途之具體例,例如可例舉:電池中之電路零件之固定用途、或上述金屬基材作為電極發揮作用之電極用途。The above-mentioned adhesive sheet can be used for known or customary purposes of bonding the adherend. Among them, the above-mentioned adhesive sheet is preferably used for adhering the adhesive layer to the insulating layer. In addition, the above-mentioned adhesive sheet is preferably used for attaching battery components, and more preferably is used for attaching all-solid-state battery components from the viewpoint of having a small total outgassing amount and excellent conductivity. Specific examples of battery member attachment applications include fixation of circuit components in batteries, or electrode applications in which the metal base material functions as an electrode.
作為上述電路零件固定用途及上述電極用途之一實施方式,例如可例舉:將上述黏著劑層貼合於聚醯亞胺膜等絕緣基板而使用之態樣,上述金屬基材作為電極發揮作用。上述電極可為正極,亦可為負極。又,上述金屬基材可附著有活性物質。例如如圖2所示,可將黏著片材1貼合於絕緣基板4(圖2(a)),以將黏著劑層3及金屬基材2切斷之方式連續形成切口L,而形成向厚度方向投影時彼此為相同形狀之包含黏著圖案及金屬圖案之圖案21(圖2(b)),繼而,將除圖案21以外之黏著劑層及金屬基材之積層體22自絕緣基板4剝離(圖2(c))。又,上述黏著劑層之黏著力藉由加熱而提高,因此可後續對上述黏著圖案進行加熱,而提高上述黏著圖案對上述絕緣基板之黏著力。 [實施例] As an embodiment of the circuit component fixing application and the electrode application, for example, the adhesive layer is bonded to an insulating substrate such as a polyimide film and used, and the metal base material functions as an electrode. . The above-mentioned electrode may be a positive electrode or a negative electrode. In addition, the above-mentioned metal base material may have an active material adhered thereto. For example, as shown in Figure 2, the adhesive sheet 1 can be bonded to the insulating substrate 4 (Figure 2(a)), and the incisions L can be continuously formed by cutting the adhesive layer 3 and the metal substrate 2 to form a direction. The pattern 21 including the adhesive pattern and the metal pattern has the same shape when projected in the thickness direction (Fig. 2(b)). Then, the laminate 22 of the adhesive layer and the metal base material other than the pattern 21 is peeled off from the insulating substrate 4. (Figure 2(c)). In addition, the adhesive force of the adhesive layer is improved by heating, so the adhesive pattern can be subsequently heated to improve the adhesive force of the adhesive pattern to the insulating substrate. [Example]
以下,例舉實施例更詳細地對本發明進行說明,但本發明並不受該等實施例之任何限定。Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited in any way by these examples.
實施例1 (聚合物A1之製備) 向具備攪拌葉片、溫度計、氮氣導入管、及冷凝器之四口燒瓶中添加丙烯酸-2-乙基己酯(2EHA)60質量份、N-乙烯基-2-吡咯啶酮(NVP)15質量份、甲基丙烯酸甲酯(MMA)10質量份、丙烯酸2-羥基乙酯(HEA)15質量份、及作為聚合溶劑之乙酸乙酯200質量份,於60℃下、氮氣氛圍下攪拌2小時後,投入作為熱聚合起始劑之2,2'-偶氮二異丁腈(AIBN)0.2質量份,於60℃下反應6小時,獲得聚合物A1之溶液。該聚合物A1之Mw為110萬,基於Fox式之Tg為-36℃。 Example 1 (Preparation of polymer A1) Add 60 parts by mass of 2-ethylhexyl acrylate (2EHA) and 15 parts by mass of N-vinyl-2-pyrrolidone (NVP) to a four-necked flask equipped with a stirring blade, a thermometer, a nitrogen gas introduction tube, and a condenser. parts, 10 parts by mass of methyl methacrylate (MMA), 15 parts by mass of 2-hydroxyethyl acrylate (HEA), and 200 parts by mass of ethyl acetate as a polymerization solvent, and stirred for 2 hours at 60°C in a nitrogen atmosphere. Then, 0.2 parts by mass of 2,2'-azobisisobutyronitrile (AIBN) as a thermal polymerization initiator was added, and the reaction was carried out at 60° C. for 6 hours to obtain a solution of polymer A1. The Mw of this polymer A1 is 1.1 million, and the Tg based on the Fox formula is -36°C.
(聚合物B1之製備) 將甲苯100質量份、甲基丙烯酸甲酯(MMA)40質量份、甲基丙烯酸丁酯(BMA)20質量份、甲基丙烯酸2-乙基己酯(2-EHMA)20質量份、官能基當量為900 g/mol之含聚有機矽氧烷骨架之甲基丙烯酸酯單體(商品名「X-22-174ASX」,信越化學工業股份有限公司製造)8.7質量份、官能基當量為4600 g/mol之含聚有機矽氧烷骨架之甲基丙烯酸酯單體(商品名「KF-2012」,信越化學工業股份有限公司製造)11.3質量份、及作為鏈轉移劑之硫代乙醇酸甲酯0.51質量份投入至具備攪拌葉片、溫度計、氮氣導入管、冷凝器、及滴液漏斗之四口燒瓶中。其次,於70℃下、氮氣氛圍下攪拌1小時後,投入作為熱聚合起始劑之AIBN 0.2質量份,於70℃下反應2小時後,投入作為熱聚合起始劑之AIBN 0.1質量份,繼而,於80℃下反應5小時,獲得聚合物B1之溶液。所獲得之聚合物B1之Mw為20000。又,聚有機矽氧烷骨架甲基丙烯酸酯單體之官能基當量(算術平均)為2990 g/mol。 (Preparation of polymer B1) 100 parts by mass of toluene, 40 parts by mass of methyl methacrylate (MMA), 20 parts by mass of butyl methacrylate (BMA), 20 parts by mass of 2-ethylhexyl methacrylate (2-EHMA), and functional groups 8.7 parts by mass of methacrylate monomer containing polyorganosiloxane skeleton (trade name "X-22-174ASX", manufactured by Shin-Etsu Chemical Industry Co., Ltd.) with an equivalent weight of 900 g/mol and a functional group equivalent of 4600 g /mol of 11.3 parts by mass of methacrylate monomer containing polyorganosiloxane skeleton (trade name "KF-2012", manufactured by Shin-Etsu Chemical Industry Co., Ltd.), and methyl thioglycolate as a chain transfer agent 0.51 parts by mass was put into a four-necked flask equipped with a stirring blade, a thermometer, a nitrogen introduction tube, a condenser, and a dropping funnel. Next, after stirring for 1 hour at 70°C in a nitrogen atmosphere, 0.2 parts by mass of AIBN as a thermal polymerization initiator was added, and after reacting at 70°C for 2 hours, 0.1 part by mass of AIBN as a thermal polymerization initiator was added. Then, the reaction was carried out at 80° C. for 5 hours to obtain a solution of polymer B1. The obtained polymer B1 had an Mw of 20,000. In addition, the functional group equivalent (arithmetic mean) of the polyorganosiloxane skeleton methacrylate monomer is 2990 g/mol.
再者,聚合物A1及聚合物B1之Mw係使用GPC裝置「HLC-8220GPC」(東曹股份有限公司製造)進行測定而算出。GPC條件如下所述。 <GPC條件> 樣品濃度:0.2 wt%(四氫呋喃(THF)溶液) 樣品注入量:10 μl 溶離液:THF 流速:0.6 ml/min 測定溫度:40℃ 管柱:樣品管柱;TSK guardcolumn SuperHZ-H(1根)+TSKgel SuperHZM-H(2根) 參考管柱;TSKgel SuperH-RC(1根) 檢測器:示差折射計(RI) In addition, Mw of polymer A1 and polymer B1 was measured using GPC apparatus "HLC-8220GPC" (manufactured by Tosoh Corporation) and calculated. GPC conditions are described below. <GPC conditions> Sample concentration: 0.2 wt% (tetrahydrofuran (THF) solution) Sample injection volume: 10 μl Eluent: THF Flow rate: 0.6 ml/min Measuring temperature: 40℃ Column: sample column; TSK guardcolumn SuperHZ-H (1 piece) + TSKgel SuperHZM-H (2 pieces) Reference column; TSKgel SuperH-RC (1 piece) Detector: Differential Refractometer (RI)
(黏著片材之製作) 向上述聚合物A1之溶液中添加相對於聚合物A1每100質量份為2.5質量份之聚合物B1、2.5質量份之異氰酸酯系交聯劑(商品名「Takenate D-110N」,三羥甲基丙烷苯二甲基二異氰酸酯,三井化學股份有限公司製造)、及1.0質量份之酚系抗氧化劑(商品名「Irganox1010」,日本巴斯夫股份有限公司製造),均勻地混合而製備黏著劑組合物。 於作為基材之厚度18 μm之電解銅箔(商品名「CF-T8G-UN-18」,福田金屬箔粉工業股份有限公司製造)上直接塗佈上述黏著劑組合物,於100℃下加熱2分鐘而進行乾燥,藉此,形成厚度9 μm之黏著劑層。於該黏著劑層之表面(黏著面)貼合剝離襯墊(商品名「MRF38」,三菱化學股份有限公司製造,聚酯膜之單面具有由矽酮系剝離處理劑獲得之剝離層的剝離襯墊,厚度38 μm)之剝離層面。以此方式獲得附剝離襯墊之黏著片材。 (Production of adhesive sheets) To the solution of the above polymer A1, 2.5 parts by mass of polymer B1 and 2.5 parts by mass of an isocyanate cross-linking agent (trade name "Takenate D-110N", trimethylol) were added per 100 parts by mass of polymer A1. Propane xylylene diisocyanate, manufactured by Mitsui Chemicals Co., Ltd.) and 1.0 parts by mass of a phenolic antioxidant (trade name "Irganox 1010", manufactured by BASF Japan Co., Ltd.) were uniformly mixed to prepare an adhesive composition. The above-mentioned adhesive composition was directly coated on an electrolytic copper foil with a thickness of 18 μm as the base material (trade name "CF-T8G-UN-18", manufactured by Futian Metal Foil Industry Co., Ltd.) and heated at 100°C. It was dried for 2 minutes, thereby forming an adhesive layer with a thickness of 9 μm. A release liner (trade name "MRF38", manufactured by Mitsubishi Chemical Co., Ltd.) is bonded to the surface (adhesive surface) of the adhesive layer. One side of the polyester film has a release layer obtained by using a silicone-based release treatment agent. Peel-off layer of liner, thickness 38 μm). In this way, an adhesive sheet with a release liner is obtained.
實施例2~3 於黏著劑組合物之製備中,如表1所示地對酚系抗氧化劑之調配量進行變更,除此以外與實施例1同樣地操作,製作黏著片材。 Examples 2-3 In the preparation of the adhesive composition, the compounding amount of the phenolic antioxidant was changed as shown in Table 1. Otherwise, the same operation as in Example 1 was performed to prepare an adhesive sheet.
實施例4 於黏著劑組合物之製備中,使用酚系抗氧化劑(商品名「Irganox565」)代替酚系抗氧化劑(商品名「Irganox1010」),除此以外與實施例2同樣地操作,製作黏著片材。 Example 4 In the preparation of the adhesive composition, a phenolic antioxidant (trade name "Irganox 565") was used instead of a phenol antioxidant (trade name "Irganox 1010"). The operation was carried out in the same manner as in Example 2 to prepare an adhesive sheet.
實施例5 使用鋁箔(軟質鋁箔,JISH4160A1N30H-0適配品,UACJ股份有限公司製造,厚度50 μm)代替電解銅箔,除此以外與實施例2同樣地操作,製作黏著片材。 Example 5 An adhesive sheet was produced in the same manner as in Example 2 except that aluminum foil (soft aluminum foil, JISH4160A1N30H-0 adapter, manufactured by UACJ Co., Ltd., thickness 50 μm) was used instead of the electrolytic copper foil.
實施例6 使用SUS(Steel Use Stainless,日本不鏽鋼標準)箔(商品名「SUS304 CSP-H」,東洋精箔股份有限公司製造,厚度40 μm)代替電解銅箔,除此以外與實施例2同樣地操作,製作黏著片材。 Example 6 The same operation as in Example 2 was performed except that SUS (Steel Use Stainless, Japanese stainless steel standard) foil (trade name "SUS304 CSP-H", manufactured by Toyo Sei Foil Co., Ltd., thickness 40 μm) was used instead of the electrolytic copper foil. Make an adhesive sheet.
比較例1~3 於黏著劑組合物之製備中,如表2所示地對酚系抗氧化劑之調配量進行變更,除此以外與實施例1同樣地操作,製作黏著片材。 Comparative examples 1 to 3 In the preparation of the adhesive composition, the compounding amount of the phenolic antioxidant was changed as shown in Table 2. Otherwise, the same operation as in Example 1 was performed to prepare an adhesive sheet.
比較例4 於黏著劑組合物之製備中,並未調配酚系抗氧化劑,除此以外與實施例1同樣地操作,製作黏著片材。 Comparative example 4 In the preparation of the adhesive composition, no phenolic antioxidant was blended. Otherwise, the same operation as in Example 1 was performed to prepare an adhesive sheet.
比較例5 於黏著劑組合物之製備中,使用磷系抗氧化劑(商品名「Irgafos 168」)代替酚系抗氧化劑(商品名「Irganox1010」),除此以外與實施例2同樣地操作,製作黏著片材。 Comparative example 5 In the preparation of the adhesive composition, a phosphorus-based antioxidant (trade name "Irgafos 168") was used instead of a phenol-based antioxidant (trade name "Irganox1010"). Otherwise, the same operation was performed as in Example 2 to prepare an adhesive sheet. .
比較例6 使用PET(polyethylene terephthalate,聚對苯二甲酸乙二酯)膜(商品名「東麗聚酯膜“Lumirror(註冊商標)”#25 S10」,東麗股份有限公司製造,厚度25 μm)代替電解銅箔,除此以外與實施例2同樣地操作,製作黏著片材。 Comparative example 6 Use PET (polyethylene terephthalate, polyethylene terephthalate) film (trade name "Toray polyester film "Lumirror (registered trademark)" #25 S10", manufactured by Toray Co., Ltd., thickness 25 μm) instead of electrolysis Except for copper foil, the same operation was performed as in Example 2 to produce an adhesive sheet.
<評價> 對實施例及比較例中所獲得之黏著片材進行以下評價。將結果示於表中。 <Evaluation> The adhesive sheets obtained in Examples and Comparative Examples were evaluated as follows. The results are shown in the table.
(1)總釋氣量 將黏著片材裁切成5 cm 2,將剝離襯墊剝離而採取試片,並封入頂空瓶中。其後,藉由頂空進樣器(HSS)於200℃下加熱60分鐘,將加熱後之氣相部分1 mL注入氣相層析儀(GC)中。其次,計算所檢測之總釋氣量。所使用之分析裝置及測定條件如下所述。 <分析裝置> HSS:Agilent Technologies,G1888 GC:Agilent Technologies,6890N <測定條件> (HSS條件) 加熱溫度:200℃ 加熱時間:60 min 樣品環路溫度:160℃ 輸送線溫度:200℃ 加壓時間:0.20 min 環路填充時間:0.20 min 環路平衡時間:0.05 min 注入時間:0.50 min (GC條件) 管柱:HP-1(0.250 mm ×30 m,df=1.0 μm) 管柱溫度:40℃(3 min)→10℃/min→120℃→20℃/min→300℃(10 min) 管柱流量:1 mL/min(He) 管柱壓力:定流量模式(81 kPa) 注入口溫度:250℃ 注入量:1 mL 注入方式:分流(20:1) 檢測器:FID(flame ionization detector,火焰離子化檢測器) 檢測器溫度:250℃ (1) Total gas release amount Cut the adhesive sheet into 5 cm 2 , peel off the release liner to obtain a test piece, and seal it in a headspace bottle. Thereafter, the sample was heated at 200°C for 60 minutes using a headspace sampler (HSS), and 1 mL of the heated gas phase was injected into the gas chromatograph (GC). Secondly, calculate the total gas release amount detected. The analysis equipment and measurement conditions used are as follows. <Analysis device> HSS: Agilent Technologies, G1888 GC: Agilent Technologies, 6890N <Measurement conditions> (HSS conditions) Heating temperature: 200°C Heating time: 60 min Sample loop temperature: 160°C Transfer line temperature: 200°C Pressurization time : 0.20 min Loop filling time: 0.20 min Loop equilibration time: 0.05 min Injection time: 0.50 min (GC conditions) Column: HP-1 (0.250 mm ×30 m, df=1.0 μm) Column temperature: 40℃(3 min)→10℃/min→120℃→20℃/min→300℃(10 min) Column flow: 1 mL/min (He) Column pressure: constant flow mode (81 kPa) Inlet temperature: 250°C Injection volume: 1 mL Injection method: split (20:1) Detector: FID (flame ionization detector, flame ionization detector) Detector temperature: 250℃
(2)180°剝離黏著力試驗 將黏著片材切割成25 mm寬者,將其作為試片。準備用甲苯清洗過之SUS板(304BA板)。其次,將黏著片材之剝離襯墊剝離,使2 kg輥往返而於SUS板貼合黏著片材之黏著面。其次,於各實施例及比較例中,分別製作於以下2個條件下放置過之黏著片材。(i)於SUS板貼合黏著片材後,於23℃之環境下放置30分鐘(初始條件)。(ii)於SUS板貼合黏著片材後,於80℃之環境下放置5分鐘後,於23℃之環境下放置30分鐘(80℃加熱後條件)。其次,對於在(i)及(ii)之條件下所製作之黏著片材,將黏著片材之另一端以300 mm/分鐘之速度向180°之剝離方向剝離,測定此時對SUS板之黏著力(阻力)(單位:N/25 mm)。 (2)180° peel adhesion test Cut the adhesive sheet into 25 mm wide and use it as a test piece. Prepare the SUS board (304BA board) cleaned with toluene. Secondly, peel off the release liner of the adhesive sheet, and make the 2 kg roller reciprocate on the SUS board to adhere to the adhesive surface of the adhesive sheet. Next, in each of the Examples and Comparative Examples, adhesive sheets placed under the following two conditions were produced. (i) After attaching the adhesive sheet to the SUS board, place it in an environment of 23°C for 30 minutes (initial conditions). (ii) After laminating the adhesive sheet to the SUS board, place it in an environment of 80°C for 5 minutes, and then place it in an environment of 23°C for 30 minutes (conditions after heating at 80°C). Secondly, for the adhesive sheet produced under the conditions (i) and (ii), peel the other end of the adhesive sheet in the peeling direction of 180° at a speed of 300 mm/min, and measure the effect on the SUS board at this time. Adhesion (resistance) (unit: N/25 mm).
(3)表面電阻值 對於黏著片材之基材表面,於溫度23℃、50%RH之氣體氛圍下,基於JIS K6911,使用URS探針,於外加電壓10 V、外加時間10秒之條件下,測定初始表面電阻值[Ω/cm 2]。作為電阻率計,使用商品名「Hiresta UP MCP-HT450型」(三菱化學股份有限公司製造)。 (3) Surface resistance value: For the base material surface of the adhesive sheet, in a gas atmosphere with a temperature of 23°C and 50% RH, based on JIS K6911, using a URS probe, under the conditions of an applied voltage of 10 V and an applied time of 10 seconds. , measure the initial surface resistance value [Ω/cm 2 ]. As a resistivity meter, a brand name "Hiresta UP MCP-HT450 type" (manufactured by Mitsubishi Chemical Co., Ltd.) was used.
[表1]
[表2]
如表中所示,實施例之黏著片材由於初始黏著力較低,且加熱後黏著力較高,因此判斷為二次加工性優異,並且黏著力隨時間上升者。又,表面電阻值較低,導電性優異。再者,儘管實施例2、5、6使用了相同之黏著劑層,但推測因金屬基材之種類或厚度等不同,而導致剝離黏著力受到金屬基材之塑性之強度差異之影響而產生差異。並且,實施例之黏著片材之總釋氣量相較於酚系抗氧化劑之含量較少之情況(比較例1~3)、不含酚系抗氧化劑之情況(比較例4)、及使用磷系抗氧化劑之情況(比較例5)有所減少。又,於使用塑膠膜作為基材之情形(比較例6)時,表面電阻值較低,導電性較差。As shown in the table, the adhesive sheet of the Example has low initial adhesive force and high adhesive force after heating, so it is judged that it has excellent secondary processability and the adhesive force increases with time. In addition, the surface resistance value is low and the conductivity is excellent. Furthermore, although the same adhesive layer was used in Examples 2, 5, and 6, it is speculated that due to the different types or thicknesses of the metal substrates, the peeling adhesive force is affected by the difference in plasticity and strength of the metal substrates. difference. In addition, the total gas release amount of the adhesive sheets of the examples is compared with the case where the content of the phenolic antioxidant is smaller (Comparative Examples 1 to 3), the case where the phenolic antioxidant is not included (Comparative Example 4), and the case where phosphorus is used. The number of antioxidants (Comparative Example 5) was reduced. In addition, when a plastic film is used as the base material (Comparative Example 6), the surface resistance value is low and the conductivity is poor.
以下,記載本發明之發明變化例。 [附記1]一種黏著片材,其具備:金屬基材、及設置於上述金屬基材之至少一面之黏著劑層,且 上述黏著劑層相對於玻璃轉移溫度未達0℃之聚合物(A)100質量份,包含聚合物(B)0.1~20質量份、及酚系抗氧化劑0.4質量份以上,該聚合物(B)包含具有聚有機矽氧烷骨架之單體(B1)及均聚物之玻璃轉移溫度為40℃以上之單體(B2)作為單體單元,並且單體(B1)之官能基當量(算術平均)為1000 g/mol以上且未達15000 g/mol,且該聚合物(B)之重量平均分子量為10000以上且未達100000。 [附記2]如附記1所記載之黏著片材,其中上述酚系抗氧化劑包含具有2個以上之酚骨架之化合物。 [附記3]如附記1或2所記載之黏著片材,其總釋氣量為15500 ppm以下。 [附記4]如附記1至3中任一項所記載之黏著片材,其用於電池構件貼附用途。 [附記5]如附記4所記載之黏著片材,其用於全固體電池構件貼附用途。 [附記6]一種全固體電池用電極,其具備:絕緣基板、上述黏著劑層貼合於上述絕緣基板而成之如附記5所記載之黏著片材、及附著於上述黏著片材中之金屬基材之活性物質。 In the following, modification examples of the present invention will be described. [Supplementary Note 1] An adhesive sheet comprising: a metal base material, and an adhesive layer provided on at least one side of the metal base material, and The above-mentioned adhesive layer contains 0.1 to 20 parts by mass of polymer (B) and more than 0.4 parts by mass of phenolic antioxidant relative to 100 parts by mass of polymer (A) whose glass transition temperature is less than 0°C. The polymer (B) ) contains a monomer (B1) with a polyorganosiloxane skeleton and a monomer (B2) with a homopolymer glass transition temperature of 40°C or above as monomer units, and the functional group equivalent of the monomer (B1) (arithmetic average) is 1000 g/mol or more and less than 15000 g/mol, and the weight average molecular weight of the polymer (B) is 10000 or more but less than 100000. [Supplement 2] The adhesive sheet according to Appendix 1, wherein the phenolic antioxidant contains a compound having two or more phenolic skeletons. [Appendix 3] For adhesive sheets as described in Appendix 1 or 2, the total gas release amount is 15,500 ppm or less. [Appendix 4] The adhesive sheet described in any one of Appendices 1 to 3 is used for attaching battery components. [Appendix 5] The adhesive sheet described in Appendix 4 is used for attaching all-solid-state battery components. [Appendix 6] An electrode for an all-solid-state battery, comprising: an insulating substrate, an adhesive sheet as described in Appendix 5 in which the adhesive layer is bonded to the insulating substrate, and a metal adhered to the adhesive sheet The active material of the base material.
1:黏著片材 2:金屬基材 3:黏著劑層 4:絕緣基材 21:圖案 22:積層體 L:切口 1: Adhesive sheet 2: Metal substrate 3: Adhesive layer 4: Insulating base material 21:Pattern 22: Laminated body L: incision
圖1係本發明之一實施方式之黏著片材之剖視模式圖。 圖2(a)~(c)係表示出使用圖1所示之黏著片材製作電極之方法之剖視模式圖。 FIG. 1 is a schematic cross-sectional view of an adhesive sheet according to one embodiment of the present invention. Figures 2 (a) to (c) are schematic cross-sectional views showing a method of producing electrodes using the adhesive sheet shown in Figure 1.
1:黏著片材 1: Adhesive sheet
2:金屬基材 2: Metal substrate
3:黏著劑層 3: Adhesive layer
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