CN113528033A - Adhesive sheet - Google Patents
Adhesive sheet Download PDFInfo
- Publication number
- CN113528033A CN113528033A CN202110428849.9A CN202110428849A CN113528033A CN 113528033 A CN113528033 A CN 113528033A CN 202110428849 A CN202110428849 A CN 202110428849A CN 113528033 A CN113528033 A CN 113528033A
- Authority
- CN
- China
- Prior art keywords
- acrylate
- meth
- adhesive sheet
- pressure
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 230000001070 adhesive effect Effects 0.000 title claims abstract description 128
- 239000000853 adhesive Substances 0.000 title claims abstract description 127
- 239000012790 adhesive layer Substances 0.000 claims abstract description 50
- 238000007373 indentation Methods 0.000 claims abstract description 27
- 239000004642 Polyimide Substances 0.000 claims abstract description 19
- 229920001721 polyimide Polymers 0.000 claims abstract description 19
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims description 92
- 239000000758 substrate Substances 0.000 claims description 44
- 239000010410 layer Substances 0.000 claims description 39
- 238000003860 storage Methods 0.000 claims description 18
- 229920000058 polyacrylate Polymers 0.000 claims description 16
- 230000009477 glass transition Effects 0.000 claims description 12
- 229920005601 base polymer Polymers 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 239000003522 acrylic cement Substances 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 85
- -1 2-ethylhexyl Chemical group 0.000 description 57
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 45
- 229920005989 resin Polymers 0.000 description 44
- 239000011347 resin Substances 0.000 description 44
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 42
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 38
- 239000003431 cross linking reagent Substances 0.000 description 38
- 239000000178 monomer Substances 0.000 description 34
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 31
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 28
- 238000011156 evaluation Methods 0.000 description 23
- 229920006243 acrylic copolymer Polymers 0.000 description 22
- 239000000243 solution Substances 0.000 description 22
- 239000012948 isocyanate Substances 0.000 description 19
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 14
- 230000008719 thickening Effects 0.000 description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 13
- 150000002513 isocyanates Chemical class 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 239000004014 plasticizer Substances 0.000 description 12
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 11
- 239000004094 surface-active agent Substances 0.000 description 11
- 229910019142 PO4 Inorganic materials 0.000 description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 10
- 239000010452 phosphate Substances 0.000 description 10
- 229920005862 polyol Polymers 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- 150000003505 terpenes Chemical class 0.000 description 9
- 235000007586 terpenes Nutrition 0.000 description 9
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000004745 nonwoven fabric Substances 0.000 description 8
- 229920000098 polyolefin Polymers 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 description 7
- 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 6
- 239000004593 Epoxy Substances 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 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 6
- 238000000576 coating method Methods 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 6
- 229920001519 homopolymer Polymers 0.000 description 6
- 239000002562 thickening agent Substances 0.000 description 6
- 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 6
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 5
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 5
- 125000000217 alkyl group Chemical group 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229920001223 polyethylene glycol Polymers 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 4
- KANZWHBYRHQMKZ-UHFFFAOYSA-N 2-ethenylpyrazine Chemical compound C=CC1=CN=CC=N1 KANZWHBYRHQMKZ-UHFFFAOYSA-N 0.000 description 4
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 4
- 239000004721 Polyphenylene oxide Substances 0.000 description 4
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229920000728 polyester Polymers 0.000 description 4
- 229920000570 polyether Polymers 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- 229920001451 polypropylene glycol Polymers 0.000 description 4
- 229960002317 succinimide Drugs 0.000 description 4
- JNPCNDJVEUEFBO-UHFFFAOYSA-N 1-butylpyrrole-2,5-dione Chemical compound CCCCN1C(=O)C=CC1=O JNPCNDJVEUEFBO-UHFFFAOYSA-N 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 125000001931 aliphatic group Chemical group 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
- 230000000694 effects Effects 0.000 description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000123 paper Substances 0.000 description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 3
- 229920002647 polyamide Polymers 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 239000004814 polyurethane Substances 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- AURYLBASVGNSON-UHFFFAOYSA-N (2,5-dioxopyrrolidin-3-ylidene)methyl prop-2-enoate Chemical compound C=CC(=O)OC=C1CC(=O)NC1=O AURYLBASVGNSON-UHFFFAOYSA-N 0.000 description 2
- IAUGBVWVWDTCJV-UHFFFAOYSA-N 1-(prop-2-enoylamino)propane-1-sulfonic acid Chemical compound CCC(S(O)(=O)=O)NC(=O)C=C IAUGBVWVWDTCJV-UHFFFAOYSA-N 0.000 description 2
- XTKZBPGQKMDFMC-UHFFFAOYSA-N 1-butyl-3-methylidenepyrrolidine-2,5-dione Chemical compound CCCCN1C(=O)CC(=C)C1=O XTKZBPGQKMDFMC-UHFFFAOYSA-N 0.000 description 2
- BQTPKSBXMONSJI-UHFFFAOYSA-N 1-cyclohexylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1CCCCC1 BQTPKSBXMONSJI-UHFFFAOYSA-N 0.000 description 2
- JWYVGKFDLWWQJX-UHFFFAOYSA-N 1-ethenylazepan-2-one Chemical compound C=CN1CCCCCC1=O JWYVGKFDLWWQJX-UHFFFAOYSA-N 0.000 description 2
- OSSNTDFYBPYIEC-UHFFFAOYSA-N 1-ethenylimidazole Chemical compound C=CN1C=CN=C1 OSSNTDFYBPYIEC-UHFFFAOYSA-N 0.000 description 2
- DCRYNQTXGUTACA-UHFFFAOYSA-N 1-ethenylpiperazine Chemical compound C=CN1CCNCC1 DCRYNQTXGUTACA-UHFFFAOYSA-N 0.000 description 2
- PBGPBHYPCGDFEZ-UHFFFAOYSA-N 1-ethenylpiperidin-2-one Chemical compound C=CN1CCCCC1=O PBGPBHYPCGDFEZ-UHFFFAOYSA-N 0.000 description 2
- BMZZOWWYEBTMBX-UHFFFAOYSA-N 1-ethyl-3-methylidenepyrrolidine-2,5-dione Chemical compound CCN1C(=O)CC(=C)C1=O BMZZOWWYEBTMBX-UHFFFAOYSA-N 0.000 description 2
- QSWFISOPXPJUCT-UHFFFAOYSA-N 1-methyl-3-methylidenepyrrolidine-2,5-dione Chemical compound CN1C(=O)CC(=C)C1=O QSWFISOPXPJUCT-UHFFFAOYSA-N 0.000 description 2
- HIDBROSJWZYGSZ-UHFFFAOYSA-N 1-phenylpyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C1=CC=CC=C1 HIDBROSJWZYGSZ-UHFFFAOYSA-N 0.000 description 2
- NQDOCLXQTQYUDH-UHFFFAOYSA-N 1-propan-2-ylpyrrole-2,5-dione Chemical compound CC(C)N1C(=O)C=CC1=O NQDOCLXQTQYUDH-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
- MZNSQRLUUXWLSB-UHFFFAOYSA-N 2-ethenyl-1h-pyrrole Chemical compound C=CC1=CC=CN1 MZNSQRLUUXWLSB-UHFFFAOYSA-N 0.000 description 2
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 description 2
- YYIOIHBNJMVSBH-UHFFFAOYSA-N 2-prop-2-enoyloxynaphthalene-1-sulfonic acid Chemical compound C1=CC=C2C(S(=O)(=O)O)=C(OC(=O)C=C)C=CC2=C1 YYIOIHBNJMVSBH-UHFFFAOYSA-N 0.000 description 2
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 description 2
- FKAWETHEYBZGSR-UHFFFAOYSA-N 3-methylidenepyrrolidine-2,5-dione Chemical compound C=C1CC(=O)NC1=O FKAWETHEYBZGSR-UHFFFAOYSA-N 0.000 description 2
- CYUZOYPRAQASLN-UHFFFAOYSA-N 3-prop-2-enoyloxypropanoic acid Chemical compound OC(=O)CCOC(=O)C=C CYUZOYPRAQASLN-UHFFFAOYSA-N 0.000 description 2
- CFZDMXAOSDDDRT-UHFFFAOYSA-N 4-ethenylmorpholine Chemical compound C=CN1CCOCC1 CFZDMXAOSDDDRT-UHFFFAOYSA-N 0.000 description 2
- JSZCJJRQCFZXCI-UHFFFAOYSA-N 6-prop-2-enoyloxyhexanoic acid Chemical compound OC(=O)CCCCCOC(=O)C=C JSZCJJRQCFZXCI-UHFFFAOYSA-N 0.000 description 2
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-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
- 239000013032 Hydrocarbon resin Substances 0.000 description 2
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- GYCMBHHDWRMZGG-UHFFFAOYSA-N Methylacrylonitrile Chemical compound CC(=C)C#N GYCMBHHDWRMZGG-UHFFFAOYSA-N 0.000 description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
- 239000004696 Poly ether ether ketone Substances 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 239000004734 Polyphenylene sulfide Substances 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 239000004760 aramid Substances 0.000 description 2
- 229920003235 aromatic polyamide Polymers 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 150000001718 carbodiimides Chemical class 0.000 description 2
- 239000013522 chelant Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 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 2
- 229920001971 elastomer Polymers 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 description 2
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- ACCCMOQWYVYDOT-UHFFFAOYSA-N hexane-1,1-diol Chemical compound CCCCCC(O)O ACCCMOQWYVYDOT-UHFFFAOYSA-N 0.000 description 2
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 229920006270 hydrocarbon resin Polymers 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- ZQXSMRAEXCEDJD-UHFFFAOYSA-N n-ethenylformamide Chemical class C=CNC=O ZQXSMRAEXCEDJD-UHFFFAOYSA-N 0.000 description 2
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 2
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 2
- 229920001707 polybutylene terephthalate Polymers 0.000 description 2
- 229920002530 polyetherether ketone Polymers 0.000 description 2
- 229920000069 polyphenylene sulfide Polymers 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical class OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- 125000005591 trimellitate group Chemical group 0.000 description 2
- 239000013638 trimer Substances 0.000 description 2
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 description 1
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 1
- 125000003837 (C1-C20) alkyl group Chemical group 0.000 description 1
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical class O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 description 1
- BPXVHIRIPLPOPT-UHFFFAOYSA-N 1,3,5-tris(2-hydroxyethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound OCCN1C(=O)N(CCO)C(=O)N(CCO)C1=O BPXVHIRIPLPOPT-UHFFFAOYSA-N 0.000 description 1
- OVBFMUAFNIIQAL-UHFFFAOYSA-N 1,4-diisocyanatobutane Chemical compound O=C=NCCCCN=C=O OVBFMUAFNIIQAL-UHFFFAOYSA-N 0.000 description 1
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 description 1
- KPAPHODVWOVUJL-UHFFFAOYSA-N 1-benzofuran;1h-indene Chemical compound C1=CC=C2CC=CC2=C1.C1=CC=C2OC=CC2=C1 KPAPHODVWOVUJL-UHFFFAOYSA-N 0.000 description 1
- BGKQCHAKBLWCDU-UHFFFAOYSA-N 1-cyclohexyl-3-methylidenepyrrolidine-2,5-dione Chemical compound O=C1C(=C)CC(=O)N1C1CCCCC1 BGKQCHAKBLWCDU-UHFFFAOYSA-N 0.000 description 1
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- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
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- 125000002958 pentadecyl 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])[H] 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
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- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920013716 polyethylene resin Polymers 0.000 description 1
- 229920000223 polyglycerol Polymers 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
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- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
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- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 description 1
- 238000004080 punching Methods 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
- 238000003756 stirring Methods 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
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- 239000000057 synthetic resin Substances 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 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
- JNXDCMUUZNIWPQ-UHFFFAOYSA-N trioctyl benzene-1,2,4-tricarboxylate Chemical compound CCCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCC)C(C(=O)OCCCCCCCC)=C1 JNXDCMUUZNIWPQ-UHFFFAOYSA-N 0.000 description 1
- 125000002948 undecyl 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])[H] 0.000 description 1
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Images
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
-
- 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
- C09J7/10—Adhesives in the form of films or foils without carriers
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Adhesive Tapes (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides an adhesive sheet which has both high-low difference following performance and stripping performance. The adhesive sheet of the present invention comprises an adhesive layer, wherein when the adhesive layer of the adhesive sheet is adhered to a Polyimide (PI) film, the adhesive strength at 23 ℃ is 2N/20mm or less, and the indentation hardness of the adhesive layer at 70 ℃ is 3MPa or less.
Description
Technical Field
The present invention relates to an adhesive sheet.
Background
In recent years, the production of various electronic components has been increasing year by year, and further, multi-functionalization and thinning have been progressing. Further, the surface irregularities of these electronic components are complicated (increased) due to the multifunctionalization. Many of these electronic components are subjected to various processes in a state of being bonded to an adhesive sheet, and shipped between processes, but when the surface shape of the electronic component is complicated, there is a problem that it is difficult to bond the adhesive sheet. In addition, with the thinning of electronic components, the risk of damaging the electronic components when the adhesive sheet is peeled increases.
In the above-mentioned applications, a pressure-sensitive adhesive sheet is sometimes used, but the pressure-sensitive adhesive sheet has a problem that it is difficult to achieve both of uneven surface following property (step following property) and light peeling. In addition, although a curable adhesive sheet may be used, there are problems such as adhesive residue due to curing failure and an increase in processes.
Documents of the prior art
Patent document
Patent document 1: japanese laid-open patent publication No. 56-61468
Disclosure of Invention
Problems to be solved by the invention
The present invention has been made to solve the above conventional problems, and an object thereof is to provide an adhesive sheet having both of step following property and peelability.
Means for solving the problems
The adhesive sheet of the present invention comprises an adhesive layer, wherein when the adhesive layer of the adhesive sheet is adhered to a Polyimide (PI) film, the adhesive strength at 23 ℃ is 2N/20mm or less, and the indentation hardness of the adhesive layer at 70 ℃ is 3MPa or less.
In one embodiment, the pressure-sensitive adhesive layer has an indentation modulus (indentation modulus) of 25MPa or more at 25 ℃.
In one embodiment, the adhesive layer includes an acrylic adhesive including an acrylic polymer as a base polymer, the acrylic polymer having a glass transition temperature of-35 ℃ or higher.
In one embodiment, the gel fraction of the pressure-sensitive adhesive layer is 70% or less.
In one embodiment, the adhesive layer has a thickness of 2 to 200 μm.
In one embodiment, the adhesive sheet further comprises a substrate, and the adhesive layer is disposed on at least one side of the substrate.
In one embodiment, the adhesive sheet has a storage modulus E' of 6 × 10 at 70 ℃7Pa or less.
In one embodiment, the thickness of the substrate is 30 to 150 μm.
ADVANTAGEOUS EFFECTS OF INVENTION
According to the present invention, a pressure-sensitive adhesive sheet having both step-following properties and peelability can be provided.
Drawings
Fig. 1(a) and (b) are schematic cross-sectional views of a pressure-sensitive adhesive sheet according to an embodiment of the present invention.
Description of the symbols
10 adhesive layer
20 base material
100. 200 adhesive sheet
Detailed Description
A. Outline of adhesive sheet
Fig. 1(a) is a schematic cross-sectional view of an adhesive sheet according to an embodiment of the present invention. The adhesive sheet 100 of the present embodiment includes an adhesive layer 10. Fig. 1(b) is a schematic cross-sectional view of an adhesive sheet according to another embodiment of the present invention. The adhesive sheet 200 of the present embodiment further includes a substrate 20, and the adhesive layer 10 is disposed on at least one side of the substrate 20.
The adhesive layer 10 has an indentation hardness of 3MPa or less at 70 ℃. When the pressure-sensitive adhesive layer of the pressure-sensitive adhesive sheet of the present invention is adhered to a Polyimide (PI) film, the adhesive strength at 23 ℃ is 2N/20mm or less. In the present invention, by setting the indentation hardness at 70 ℃ and the adhesive force at 23 ℃ to the above ranges, a pressure-sensitive adhesive sheet having excellent both step following properties and peeling properties can be obtained. More specifically, when the adhesive sheet is adhered to a predetermined adherend at a high temperature, the adhesive sheet of the present invention has desirable flexibility (flexibility close to that of the pressure-sensitive adhesive layer), excellent workability, and excellent conformability to the uneven surface of the adherend having the uneven surface. On the other hand, when peeled off at room temperature, the adhesive sheet of the present invention can have high elasticity (for example, can have mechanical properties such as a UV-curable adhesive layer), can exhibit excellent peelability, and can prevent adhesive residue. The pressure-sensitive adhesive layer having the above-described characteristics can be obtained, for example, by adjusting the composition of the pressure-sensitive adhesive constituting the pressure-sensitive adhesive layer, adjusting the gel fraction of the pressure-sensitive adhesive layer, and the like (details will be described later).
When the pressure-sensitive adhesive layer of the pressure-sensitive adhesive sheet of the invention is adhered to a Polyimide (PI) film, the adhesive strength at 23 ℃ is preferably 0.05N/20mm to 2N/20mm, more preferably 0.10N/20mm to 1.50N/20mm, still more preferably 0.15N/20mm to 1.50N/20mm, and particularly preferably 0.15N/20mm to 1.25N/20 mm. In the present specification, the adhesive force is an adhesive force measured under a condition of a tensile rate of 10m/min and a peel angle of 180 ° at 23 ℃ using an evaluation sample obtained by pressing an adhesive sheet having a width of 20mm × a length of 100mm against the surface of a PI film using a heated roll laminator at a roll temperature of 80 ℃, a roll pressure of 0.2MPa and a roll speed of 0.5m/min, standing the pressure-sensitive adhesive sheet at 23 ℃ for 30 minutes in a 50% RH environment, and then storing the pressure-sensitive adhesive sheet at 40 ℃ for 48 hours.
The thickness of the pressure-sensitive adhesive sheet of the present invention is preferably 30 μm to 500 μm, more preferably 40 μm to 300 μm.
The storage modulus E' of the adhesive sheet of the invention at 70 ℃ is preferably 6X 107Pa or less, more preferably 5X 107Pa or less, more preferably 4.5X 107Pa or less, particularly preferably 4X 107Pa or less. Within such a range, a pressure-sensitive adhesive sheet having excellent step following properties and excellent sticking workability can be obtained. The pressure-sensitive adhesive sheet having a storage modulus E' in the above range can be obtained, for example, by a configuration including a substrate. The lower limit of the storage modulus E' of the adhesive sheet at 70 ℃ is, for example, 0.5X 107Pa (preferably 1X 10)7Pa) is added. The storage modulus E' is measured as described later.
The storage modulus E' of the adhesive sheet of the invention at 23 ℃ is preferably 1.0X 106Pa～1.0×1010Pa, more preferably 1.0X 107Pa～1.0×1010Pa, more preferably 1.0X 107Pa～1.0×109Pa。
The pressure-sensitive adhesive sheet may further include any appropriate layer in addition to the pressure-sensitive adhesive layer and the substrate. For example, the pressure-sensitive adhesive layer may further include another pressure-sensitive adhesive layer in addition to the above pressure-sensitive adhesive layer. More specifically, examples of the structure of the pressure-sensitive adhesive sheet of the present invention include: (i) a pressure-sensitive adhesive layer single layer, (ii) a structure formed of a pressure-sensitive adhesive layer and a substrate, (iii) a structure including a pressure-sensitive adhesive layer, a substrate, and a pressure-sensitive adhesive layer in this order, (iv) a structure including a pressure-sensitive adhesive layer, a substrate, and another pressure-sensitive adhesive layer in this order, and the like. Other adhesive layers may be of known construction. In addition, any suitable release liner may be disposed on the surface of the pressure-sensitive adhesive layer until the pressure-sensitive adhesive layer is used, in order to protect the surface.
B. Adhesive layer
As described above, the indentation hardness of the adhesive layer at 70 ℃ is 3MPa or less. The indentation hardness of the pressure-sensitive adhesive layer at 70 ℃ is preferably 1.5MPa or less, more preferably 1MPa or less, and still more preferably 0.5MPa or less. Within such a range, a pressure-sensitive adhesive sheet having excellent step following properties and excellent sticking workability can be obtained. The lower limit of the indentation hardness of the adhesive layer at 70 ℃ is, for example, 0.02 MPa. The indentation hardness is measured as described later.
The pressure-sensitive adhesive layer preferably has an indentation modulus at 25 ℃ of 10MPa or more, more preferably 20MPa, and still more preferably 25MPa or more. Within such a range, a pressure-sensitive adhesive sheet exhibiting excellent peelability and capable of significantly preventing the adherend from being damaged can be obtained. Further, a pressure-sensitive adhesive sheet with less adhesive residue can be provided.
The ratio (H1/H2) of the indentation hardness H1 of the adhesive layer at 70 ℃ to the indentation modulus H2 at 25 ℃ is preferably 5.0X 10-2The following, more preferably 5.0X 10-3The following. In such a range, the effect of the present invention becomes more remarkable. The lower limit of H1/H2 is, for example, 1.0X 10-5。
The thickness of the pressure-sensitive adhesive layer is preferably 2 to 200. mu.m, more preferably 5 to 150. mu.m, and still more preferably 5 to 120. mu.m. When the content is in such a range, a pressure-sensitive adhesive sheet having excellent adhesive strength and excellent productivity can be obtained.
The gel fraction of the pressure-sensitive adhesive layer is preferably 70% or less, more preferably 65% or less, and still more preferably 50% or less. In the case where the elastic modulus is in such a range, a pressure-sensitive adhesive layer with a well-adjusted elastic modulus can be formed, and as a result, a pressure-sensitive adhesive sheet with excellent step-following properties and excellent sticking workability can be obtained. The lower limit of the gel fraction of the adhesive layer is, for example, 10%. The gel fraction is measured as described later.
Typically, the adhesive layer contains an adhesive for imparting adhesiveness. As the binder, any suitable binder may be used as long as the effects of the present invention can be obtained. Examples of the binder include: acrylic adhesives, silicone adhesives, vinyl alkyl ether adhesives, polyester adhesives, polyamide adhesives, urethane adhesives, fluorine-containing adhesives, styrene-diene block copolymer adhesives, active energy ray-curable adhesives, and the like. Among them, acrylic adhesives are preferable.
The acrylic adhesive may be an adhesive containing an acrylic polymer as a base polymer. Examples of the adhesive include an acrylic adhesive containing an acrylic polymer (homopolymer or copolymer) as a base polymer, the acrylic polymer containing 1 or 2 or more kinds of alkyl (meth) acrylates as monomer components. Specific examples of the alkyl (meth) acrylate include: methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, isopropyl (meth) acrylate, butyl (meth) acrylate, isobutyl (meth) acrylate, sec-butyl (meth) acrylate, tert-butyl (meth) acrylate, pentyl (meth) acrylate, hexyl (meth) acrylate, heptyl (meth) acrylate, octyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, isooctyl (meth) acrylate, nonyl (meth) acrylate, isononyl (meth) acrylate, decyl (meth) acrylate, isodecyl (meth) acrylate, undecyl (meth) acrylate, dodecyl (meth) acrylate, tridecyl (meth) acrylate, tetradecyl (meth) acrylate, pentadecyl (meth) acrylate, dodecyl (meth) acrylate, and the like, C1-20 alkyl (meth) acrylates such as cetyl (meth) acrylate, heptadecyl (meth) acrylate, octadecyl (meth) acrylate, nonadecyl (meth) acrylate, and eicosyl (meth) acrylate. Among them, alkyl (meth) acrylates having a linear or branched alkyl group having 4 to 18 carbon atoms can be preferably used.
For the purpose of cohesive force, heat resistance and crosslinkingAnd the like, and the acrylic polymer may contain units corresponding to other monomer components copolymerizable with the alkyl (meth) acrylate, if necessary. Examples of such monomer components include: carboxyl group-containing monomers such as acrylic acid, methacrylic acid, carboxyethyl acrylate, carboxypentyl acrylate, itaconic acid, maleic acid, fumaric acid, and crotonic acid; anhydride monomers such as maleic anhydride and itaconic anhydride; hydroxyl-containing monomers such as hydroxyethyl (meth) acrylate, hydroxypropyl (meth) acrylate, hydroxybutyl (meth) acrylate, hydroxyhexyl (meth) acrylate, hydroxyoctyl (meth) acrylate, hydroxydecyl (meth) acrylate, hydroxylauryl (meth) acrylate, and 4-hydroxymethylcyclohexyl (meth) methyl methacrylate, sulfonic acid group-containing monomers such as styrenesulfonic acid, allylsulfonic acid, 2- (meth) acrylamide-2-methylpropanesulfonic acid, metha) acrylamidopropanesulfonic acid, sulfopropyl (meth) acrylate, and (meth) acryloyloxynaphthalenesulfonic acid, N-substituted amide monomers such as (meth) acrylamide, N-dimethyl (meth) acrylamide, N-butyl (meth) acrylamide, N-hydroxymethyl (meth) acrylamide, and N-hydroxymethylpropane (meth) acrylamide, aminoethyl (meth) acrylate, hydroxyethyl (meth) acrylate, hydroxyhexyl (meth) acrylate, hydroxyoctyl (meth) acrylate, allylsulfonic acid group-containing monomers such as styrenesulfonic acid, 2- (meth) acrylamidopropanesulfonic acid, sulfopropyl (meth) acrylate, and sulfo (meth) acryloyloxynaphthalenesulfonic acid, Aminoalkyl (meth) acrylate monomers such as N, N-dimethylaminoethyl (meth) acrylate and t-butylaminoethyl (meth) acrylate; alkoxyalkyl (meth) acrylate monomers such as methoxyethyl (meth) acrylate and ethoxyethyl (meth) acrylate; maleimide monomers such as N-cyclohexylmaleimide, N-isopropylmaleimide, N-laurylmaleimide and N-phenylmaleimide; itaconimide monomers such as N-methylitaconimide, N-ethylitaconimide, N-butylitaconimide, N-octylitaconimide, N-2-ethylhexyl itaconimide, N-cyclohexylitaconimide and N-laurylitaconimide; succinimide monomers such as N- (meth) acryloyloxymethylene succinimide, N- (meth) acryloyl-6-oxyhexamethylene succinimide, and N- (meth) acryloyl-8-oxyoctamethylene succinimide; vinyl acetate, vinyl propionate, N-vinylpyrrolidone, methylvinylpyrrolidone, vinylpyridine, vinylpiperidone, vinylpyrimidinePyridine, vinyl piperazine, vinyl pyrazine, vinyl pyrrole, vinyl imidazole, vinyl
Vinyl monomers such as oxazole, vinyl morpholine, N-vinylcarboxylic acid amides, styrene, alpha-methylstyrene, and N-vinylcaprolactam; cyanoacrylate monomers such as acrylonitrile and methacrylonitrile; epoxy group-containing acrylic monomers such as glycidyl (meth) acrylate; glycol acrylate monomers such as polyethylene glycol (meth) acrylate, polypropylene glycol (meth) acrylate, methoxyethylene glycol (meth) acrylate, and methoxypolypropylene glycol (meth) acrylate; acrylic ester monomers having a heterocyclic ring, a halogen atom, a silicon atom, and the like, such as tetrahydrofurfuryl (meth) acrylate, fluorine-containing (meth) acrylate, and silicone (meth) acrylate; polyfunctional monomers such as hexanediol di (meth) acrylate, (poly) ethylene glycol di (meth) acrylate, (poly) propylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate, pentaerythritol di (meth) acrylate, trimethylolpropane tri (meth) acrylate, pentaerythritol tri (meth) acrylate, dipentaerythritol hexa (meth) acrylate, epoxy acrylate, polyester acrylate, and urethane acrylate; olefin monomers such as isoprene, butadiene, and isobutylene; vinyl ether monomers such as vinyl ether. These monomer components may be used alone or in combination of 2 or more.
The glass transition temperature Tg of the acrylic polymer is preferably-35 ℃ or higher, more preferably-30 to 50 ℃, and still more preferably-30 to 30 ℃. When a polymer having a high glass transition temperature is used, a highly elastic adhesive layer can be formed. The pressure-sensitive adhesive sheet having such a pressure-sensitive adhesive layer exhibits excellent peelability and can significantly prevent the adherend from being damaged. Further, the pressure-sensitive adhesive sheet is also advantageous in that the adhesive residue is small. When the acrylic polymer is a copolymer, the glass transition temperature is determined by the Fox equation. The calculated Fox is the glass transition temperature Tg (. degree.C.) of the copolymer and the monomer components constituting the copolymer, as shown belowGlass transition temperature Tg of homopolymer obtained by homopolymerizationiIn (. degree. C.) relationship. In the following Fox formula, Tg (. degree. C.) represents the glass transition temperature of the copolymer, and W representsiDenotes the weight fraction of monomer i, Tgi(° c) denotes the glass transition temperature of a homopolymer formed from monomer i.
1/(273+Tg)＝Σ(Wi/(273+Tgi))
As the glass transition temperature of a homopolymer formed from monomers, the value described in "Polymer Handbook" (4 th edition, John Wiley & Sons, Inc, 1999) can be used. When a plurality of Tg values are described in this document, "conditional" is used.
The acrylic polymer preferably contains a structural unit derived from a monomer a having a glass transition temperature (Tg) of-20 ℃ or higher (preferably 0 ℃ or higher, more preferably 20 ℃ or higher) when forming a homopolymer. In the acrylic polymer, the content of the structural unit derived from the monomer a is preferably 20 parts by weight or more, more preferably 30 parts by weight or more, and still more preferably 40 to 80 parts by weight, based on 100 parts by weight of the acrylic polymer.
Specific examples of the monomer a include: methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, isopropyl (meth) acrylate, butyl (meth) acrylate, isobutyl (meth) acrylate, sec-butyl (meth) acrylate, tert-butyl (meth) acrylate, pentyl (meth) acrylate, hexyl (meth) acrylate, heptyl (meth) acrylate, acrylic acid, methacrylic acid, carboxyethyl acrylate, carboxypentyl acrylate, hydroxybutyl (meth) acrylate, hydroxyhexyl (meth) acrylate, N-cyclohexylmaleimide, N-isopropylmaleimide, N-phenylmaleimide, N-methylitaconimide, N-ethylitaconimide, N-butylitaconimide, N- (meth) acryloyloxymethylene succinimide, N-butylmaleimide, N- (meth) acrylic acid, N-butylmaleimide, and the like, N-butylmaleimide, and the like, N- (meth) acryloyl-6-oxy-hexamethylene succinimide, vinyl acetate, vinyl propionate, N-vinylpyrrolidone, methylvinylpyrazinePyrrolidone, vinylpyridine, vinylpiperidone, vinylpyrimidine, vinylpiperazine, vinylpyrazine, vinylpyrrole, vinylimidazole, vinyl
Oxazole, vinyl morpholine, N-vinyl carboxylic acid amides, styrene, α -methylstyrene, N-vinyl caprolactam, acrylonitrile, methacrylonitrile, (meth) acrylic acid polyethylene glycol, (meth) acrylic acid polypropylene glycol, hexanediol di (meth) acrylate, (poly) ethylene glycol di (meth) acrylate, (poly) propylene glycol di (meth) acrylate, isoprene, butadiene, isobutylene and the like.
The binder may contain any suitable additive as required. Examples of such additives include: crosslinking agents, thickeners, plasticizers, pigments, dyes, fillers, anti-aging agents, conductive materials, antistatic agents, ultraviolet absorbers, light stabilizers, release modifiers, softeners, surfactants, flame retardants, antioxidants, and the like.
As the thickener, any suitable thickener can be used. As the thickener, for example, a thickening resin can be used. Specific examples of the thickening resin include: rosin-based thickening resins (e.g., unmodified rosin, modified rosin, rosin phenol-based resin, rosin ester-based resin, etc.), terpene-based thickening resins (e.g., terpene-based resin, terpene phenol-based resin, styrene-modified terpene-based resin, aromatic-modified terpene-based resin, hydrogenated terpene-based resin), hydrocarbon-based thickening resins (e.g., aliphatic hydrocarbon resin, aliphatic cyclic hydrocarbon resin, aromatic hydrocarbon resin (e.g., styrene-based resin, xylene-based resin, etc.), aliphatic/aromatic petroleum resin, aliphatic/alicyclic petroleum resin, hydrogenated hydrocarbon resin, coumarone-based resin, coumarone indene-based resin, etc.), phenol-based thickening resins (e.g., alkyl phenol-based resin, xylene formaldehyde-based resin, resol, phenol varnish, etc.), ketone-based thickening resins, polyamide-based thickening resins, terpene-based resins (e.g., terpene-based resin, styrene-based resin, aromatic hydrocarbon-based resin, hydrogenated hydrocarbon-based resin, coumarone-based resin, etc.), phenol-based thickening resins, and the like, Epoxy-based thickening resins, elastomer-based thickening resins, and the like. Among them, rosin-based thickening resins, terpene-based thickening resins, or hydrocarbon-based thickening resins (styrene-based resins, etc.) are preferable. The thickener may be used alone, or in combination of 2 or more.
The amount of the thickener added is preferably 0.2 to 100 parts by weight, more preferably 1 to 50 parts by weight, based on 100 parts by weight of the base polymer.
Examples of the crosslinking agent include: isocyanate crosslinking agents, epoxy crosslinking agents, melamine crosslinking agents, peroxide crosslinking agents, urea crosslinking agents, metal alkoxide crosslinking agents, metal chelate crosslinking agents, metal salt crosslinking agents, carbodiimide crosslinking agents, urea crosslinking agents, metal alkoxide crosslinking agents, metal chelate crosslinking agents, metal salt crosslinking agents, carbodiimide crosslinking agents, and the like,
Oxazoline crosslinking agents, aziridine crosslinking agents, amine crosslinking agents, and the like. Among them, an isocyanate-based crosslinking agent or an epoxy-based crosslinking agent is preferable. The gel fraction of the adhesive layer can be adjusted by the kind and amount of the crosslinking agent added.
Specific examples of the isocyanate-based crosslinking agent include: lower aliphatic polyisocyanates such as butylene diisocyanate and hexamethylene diisocyanate; alicyclic isocyanates such as cyclopentylene diisocyanate, cyclohexylene diisocyanate and isophorone diisocyanate; aromatic isocyanates such as 2, 4-tolylene diisocyanate, 4' -diphenylmethane diisocyanate, and xylylene diisocyanate; isocyanate adducts such as trimethylolpropane/tolylene diisocyanate trimer adduct (product name "Coronate L" manufactured by japan polyurethane industries co., ltd.), trimethylolpropane/hexamethylene diisocyanate trimer adduct (product name "Coronate HL" manufactured by japan polyurethane industries co., ltd.), isocyanurate body of hexamethylene diisocyanate (product name "Coronate HX" manufactured by japan polyurethane industries co., ltd.); and so on. The content of the isocyanate-based crosslinking agent may be set to any appropriate amount depending on the desired adhesive strength, elasticity of the pressure-sensitive adhesive layer, and the like, and is typically 0.1 to 20 parts by weight, more preferably 0.5 to 10 parts by weight, based on 100 parts by weight of the base polymer.
Examples of the epoxy crosslinking agent include: n, N, N ', N' -tetraglycidyl m-xylylenediamine, diglycidylaniline, 1, 3-bis (N, N-glycidylaminomethyl) cyclohexane (trade name "TETRAD C" manufactured by Mitsubishi gas chemical Co., Ltd.), 1, 6-hexanediol diglycidyl ether (trade name "Eplight 1600" manufactured by Co., Ltd.), neopentyl glycol diglycidyl ether (trade name "Eplight 1500 NP" manufactured by Co., Ltd.), ethylene glycol diglycidyl ether (trade name "Eplight 40E" manufactured by Co., Ltd.), propylene glycol diglycidyl ether (trade name "Eplight 70P" manufactured by Co., Ltd.), polyethylene glycol diglycidyl ether (trade name "EPE-400" manufactured by Japan oil and fat Co., Ltd.), "IOL"), Polypropylene glycol diglycidyl ether (trade name "EPIOL P-200" manufactured by japan fat and oil co., ltd.), sorbitol polyglycidyl ether (trade name "denanol EX-611" manufactured by Nagase ChemteX), glycerol polyglycidyl ether (trade name "denanol EX-314" manufactured by Nagase chemtx), pentaerythritol polyglycidyl ether, polyglycerol polyglycidyl ether (trade name "denanol EX-512" manufactured by nage ChemteX), sorbitan polyglycidyl ether, trimethylolpropane polyglycidyl ether, adipic acid diglycidyl ester, phthalic acid diglycidyl ester, triglycidyl tris (2-hydroxyethyl) isocyanurate, resorcinol diglycidyl ether, bisphenol S diglycidyl ether, epoxy resins having 2 or more epoxy groups in the molecule, and the like. The content of the epoxy crosslinking agent may be set to any appropriate amount depending on the desired adhesive strength, elasticity of the adhesive layer, and the like, and is typically 0.01 to 10 parts by weight, more preferably 0.03 to 5 parts by weight, based on 100 parts by weight of the base polymer.
As the plasticizer, any suitable plasticizer can be used. Specific examples of the plasticizer include: trimellitate plasticizers, pyromellitic acid esters plasticizers, polyester plasticizers, adipic acid plasticizers, and the like. Among them, preferred are trimellitate plasticizers (e.g., tri-n-octyl trimellitate, tri-2-ethylhexyl trimellitate, etc.) and pyromellitic acid ester plasticizers (e.g., tetra-n-octyl pyromellitate, tetra-2-ethylhexyl pyromellitate, etc.). The plasticizer may be used alone, or 2 or more kinds may be used in combination. The content of the plasticizer is preferably 0.1 to 20 parts by weight, more preferably 1 to 5 parts by weight, based on 100 parts by weight of the base polymer.
C. Base material
Examples of the substrate include: a resin sheet, a nonwoven fabric, paper, a metal foil, a woven fabric, a rubber sheet, a foamed sheet, a laminate of these (particularly a laminate containing a resin sheet), and the like. Examples of the resin constituting the resin sheet include: polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polybutylene terephthalate (PBT), Polyethylene (PE), polypropylene (PP), ethylene-propylene copolymer, ethylene-vinyl acetate copolymer (EVA), polyamide (nylon), wholly aromatic polyamide (aramid), Polyimide (PI), polyvinyl chloride (PVC), Polyphenylene Sulfide (PPs), fluorine-containing resin, polyether ether ketone (PEEK), and the like. Examples of the nonwoven fabric include: nonwoven fabrics made of heat-resistant natural fibers, such as nonwoven fabrics containing abaca; and synthetic resin nonwoven fabrics such as polypropylene resin nonwoven fabrics, polyethylene resin nonwoven fabrics, and ester resin nonwoven fabrics. As the metal foil, there can be mentioned: copper foil, stainless steel foil, aluminum foil, and the like. As the paper, there can be mentioned: japanese paper, kraft paper, and the like.
The thickness of the substrate may be set to any appropriate thickness according to the desired strength, flexibility, use purpose, and the like. The thickness of the substrate is preferably 30 to 150. mu.m, more preferably 50 to 100. mu.m. Within such a range, a pressure-sensitive adhesive sheet having excellent step following properties and excellent sticking workability can be obtained.
The storage modulus E' of the above-mentioned substrate at 70 ℃ is preferably 6X 107Pa or less, more preferably 5X 107Pa or less, more preferably 4.5X 107Pa or less, particularly preferably 4X 107Pa or less. Within such a range, excellent step followability and excellent sticking workability can be obtainedA pressure-sensitive adhesive sheet. The lower limit of the storage modulus E' of the above-mentioned base material at 70 ℃ is, for example, 0.5X 107Pa (preferably 1X 10)7Pa)。
The storage modulus E' of the above-mentioned substrate at 23 ℃ is 1.0X 106Pa～1.0×1010Pa, more preferably 1.0X 107Pa～1.0×1010Pa, more preferably 1.0X 107Pa～1.0×109Pa。
The substrate may be surface-treated. Examples of the surface treatment include: corona treatment, chromic acid treatment, ozone exposure, flame exposure, high-voltage electric shock exposure, ionizing radiation treatment, coating treatment with a primer, and the like.
Examples of the organic coating material include those described in plastic hard coat material II (CMC published, (2004)). The urethane polymer is preferably used, and more preferably, a polyacrylic urethane, a polyester urethane, or a precursor thereof is used, because they are easy to apply/coat a substrate, and are industrially available at low cost by various options. The urethane-based polymer is, for example, a polymer comprising a reaction mixture of an isocyanate monomer and an alcoholic hydroxyl group-containing monomer (for example, a hydroxyl group-containing acrylic compound or a hydroxyl group-containing ester compound). The organic coating material may contain a chain extender such as polyamine, an antioxidant, an oxidation stabilizer, and the like as optional additives. The thickness of the organic coating layer is not particularly limited, and is suitably, for example, about 0.1 to 10 μm, preferably about 0.1 to 5 μm, and more preferably about 0.5 to 5 μm.
D. Method for producing adhesive sheet
The adhesive sheet of the present invention can be produced by any suitable method. Examples of the method for producing the pressure-sensitive adhesive sheet of the present invention include: a method of directly applying an adhesive composition to a substrate (to an arbitrary appropriate substrate when obtaining an adhesive sheet not including a substrate), a method of transferring a coating layer formed by applying an adhesive composition to an arbitrary appropriate substrate to a substrate, or the like. The adhesive composition may comprise any suitable solvent.
As the method for applying the adhesive composition, any suitable application method can be used. For example, each layer may be formed by drying after coating. Examples of the coating method include: a coating method using a multilayer coater, die coater, gravure coater, or the like. Examples of the drying method include natural drying and heat drying. The heating temperature in the heat drying may be set to any appropriate temperature according to the characteristics of the substance to be dried.
Matters disclosed in the present specification include the following embodiments.
(1) The adhesive sheet of the present invention comprises an adhesive layer, wherein when the adhesive layer of the adhesive sheet is adhered to a Polyimide (PI) film, the adhesive strength at 23 ℃ is 2N/20mm or less, and the indentation hardness of the adhesive layer at 70 ℃ is 3MPa or less.
(2) In one embodiment, the pressure-sensitive adhesive layer has an indentation modulus at 25 ℃ of 25MPa or more.
(3) In one embodiment, the adhesive layer includes an acrylic adhesive including an acrylic polymer as a base polymer, the acrylic polymer having a glass transition temperature of-35 ℃ or higher.
(4) In one embodiment, the gel fraction of the pressure-sensitive adhesive layer is 70% or less.
(5) In one embodiment, the adhesive layer has a thickness of 2 to 200 μm.
(6a) In one embodiment, the adhesive sheet comprises a single adhesive layer.
(6b-1) in one embodiment, the adhesive sheet further comprises a substrate, and the adhesive layer is disposed on at least one side of the substrate.
(6b-2) in one embodiment, the pressure-sensitive adhesive sheet has a structure comprising a pressure-sensitive adhesive layer and a substrate.
(6b-3) in one embodiment, the pressure-sensitive adhesive sheet has a structure comprising a pressure-sensitive adhesive layer, a substrate and a pressure-sensitive adhesive layer in this order.
(6b-4) in one embodiment, the pressure-sensitive adhesive sheet has a structure comprising a pressure-sensitive adhesive layer, a substrate, and another pressure-sensitive adhesive layer in this order.
(7) In one embodiment, the adhesive sheet has a storage modulus E' of 6 × 10 at 70 ℃7Pa or less.
(8) In one embodiment, the thickness of the substrate is 30 to 150 μm.
(9) In one embodiment, the adhesive sheet has a thickness of 30 to 500 μm.
(10) In one embodiment, the adhesive sheet has a storage modulus E' of 1.0 × 10 at 23 ℃6Pa～1.0×1010Pa。
(11) In one embodiment, the acrylic polymer contained in the acrylic adhesive contains a structural unit derived from a monomer a having a glass transition temperature (Tg) of-20 ℃ or higher when forming a homopolymer.
(12) In one embodiment, the monomer a is butyl (meth) acrylate.
(13) In one embodiment, the substrate has a storage modulus E' of 6X 10 at 70 ℃7Pa or less.
(14) In one embodiment, the storage modulus E' of the above substrate at 23 ℃ is 1.0X 106Pa～1.0×1010Pa。
Examples
The present invention will be specifically described below with reference to examples, but the present invention is not limited to these examples. The evaluation methods in the examples are as follows. In the following evaluation, a pressure-sensitive adhesive sheet obtained by peeling off a separator was used. In the examples, "part(s)" and "%" are based on weight unless otherwise specified.
(1) Indentation hardness/modulus of elasticity
The pressure-sensitive adhesive layer was subjected to a press-in test under the following conditions, and the indentation hardness was determined from the result.
(measurement apparatus and measurement conditions)
The device comprises the following steps: tribo Inder manufactured by Hysitron corporation
Using a pressure head: conical (spherical indenter: radius of curvature 10 μm)
The determination method comprises the following steps: single indentation assay
Measuring temperature: 25 ℃ and 70 DEG C
Setting the pressing depth: about 1000nm
Pressing-in speed: about 500nm/sec
Measuring the gas atmosphere: in the air
(indentation hardness/indentation modulus measuring method at 70 ℃ C.)
Using the apparatus described above, after a given heating process (elevated from room temperature (25 ℃) to 70 ℃ and held for 1 hour), a Conical-type diamond indenter was pressed vertically into the sample to a depth of 1000nm from the surface. The indentation hardness of the surface was determined from the displacement, load and theoretically calculated indentation area obtained when the indenter was pressed in, using the analytical software, Triboscan ver.9.2.12.0. Further, using the software described above, the elastic modulus of the surface was determined from the displacement obtained after removing the indenter, the load, and the indentation area theoretically calculated.
(method of measuring indentation hardness/elastic modulus at 25 ℃ C.)
The indentation hardness and the elastic modulus of the adhesive layer were measured in the same manner as described above except that the heating process was not performed (Oliver-Pharr method).
(2) Storage modulus E 'of adhesive sheet'
A sample for evaluation was obtained by punching the adhesive sheet to a width of 5 mm. times.a length of 70 mm.
The storage modulus E' at 70 ℃ was measured using a dynamic viscoelasticity measuring apparatus (RSA-G2, TA-instruments Co., Ltd.) at a frequency of 1Hz and a crosshead of 20 mm. The storage modulus E 'of the adhesive sheet depends on the characteristics of the substrate, and therefore, the thickness information for calculating the storage modulus E' uses the value of the substrate thickness of the adhesive sheet. The thickness of the base material of the pressure-sensitive adhesive sheet was confirmed by observation from the sheet cross-sectional direction.
(3) Adhesive force
An adhesive sheet having a width of 20mm and a length of 100mm was rolled using a heated roll laminator (manufactured by MCK corporation, modified MRK-600A)The temperature was 80 ℃, the roll pressure was 0.2MPa, and the roll speed was 0.5m/min, and the temperature was pressed against the surface of a PI film (product of Kapton 200V 50 μm, manufactured by DuPont Toray Co.), and then the PI film was left to stand in an atmosphere of 23 ℃ and 50% RH for 30 minutes, and then the PI film was stored in an atmosphere of 40 ℃ for 48 hours, and the tensile rate was 10m/min, and the peel angle was measured under 180 ℃ conditions using the obtained evaluation sample in an atmosphere of 23 ℃. Further, the adhesive sheet (comparative example 5) using the UV-curable adhesive was irradiated at an illuminance of 450mJ/cm2The adhesive was cured by irradiating UV light having a wavelength of 355nm, and then the adhesive force was measured in the same manner as described above. In the measurement of the adhesive force, a high-speed peel adhesion force measuring instrument (manufactured by TESTER SANGYO) was used to cut 10% of the start and end of the measurement range, and the average value of the adhesive force in the other ranges was read.
(4) Following property of height difference
An adhesive sheet 20mm wide by 100mm long was pressure-bonded to the matte surface of matte treated PET (EMBLET SM-38D, manufactured by Unitika Co.) and the film surface of a PET film (Lumiror S10#38, manufactured by Toray Co.) by reciprocating a 2kg roller 1 time in an air atmosphere at 80 ℃. Then, the adhesive strength to a matte side of PET (M1) and the adhesive strength to a smooth side of PET (F1) were measured at a tensile speed of 0.3M/min and a tensile angle of 180 ℃ by using a tensile tester (AUTOGRAPH, manufactured by Shimadzu corporation). Then, the ratio (T) (T — M1/F1) of (M1) to (F1) was calculated, and the adhesive concave-convex following property was evaluated.
O: an adhesive force ratio (T) of 0.5 or more
X: the adhesion ratio (T) is less than 0.5
(5) Residual adhesive property
An adhesive sheet having a width of 20mm × a length of 100mm was pressure-bonded to the surface of a PI film (Kapton 200V 50 μm product, manufactured by DuPont Toray) using a heated roll laminator (modified MRK-600A, manufactured by MCK) at a roll temperature of 80 ℃, a roll pressure of 0.2MPa, and a roll speed of 0.5m/min, and then left to stand at 23 ℃ and 50% RH for 30 minutes, and then stored at 40 ℃ for 48 hours, and the sheet was peeled off using the obtained evaluation sample at a stretching speed of 10m/min and a peeling angle of 180 °, and the presence or absence of residual adhesive was confirmed visually. Further, the adhesive sheet using the UV curable adhesive was irradiated at an illuminance of 450mJ/cm2After curing the adhesive by irradiation with UV light having a wavelength of 355nm, the adhesive sheet was peeled off in the same manner as described above, and the presence or absence of adhesive residue was visually confirmed.
O: no adhesive residue
X: with residual glue
(6) Adhesive gel fraction
100mg of the adhesive layer was collected, wrapped with a 5cm square PTFE film, and then immersed in 50ml of ethyl acetate, followed by stirring with a shaker for 2 days. Then, the ethyl acetate was removed, and an unnecessary amount of ethyl acetate was dried and the dried product was weighed. The gel fraction (%) was determined by the formula [ (weight of ethyl acetate-insoluble matter)/(weight of sample before ethyl acetate impregnation) ] × 100.
[ example 1]
AN ethyl acetate solution containing 100 parts by weight of AN acrylic copolymer (butyl acrylate (BA)/Acrylonitrile (AN)/Acrylic Acid (AA) (weight ratio) 72/27/1, weight average molecular weight: 800000), 0.25 parts by weight of ethylenediamine polyol (ADEKA EDP-300, manufactured by ADEKA corporation), 0.50 parts by weight of AN isocyanate-based crosslinking agent (Coronate L, manufactured by tokyo co., ltd.), and 0.5 parts by weight of a phosphate-based surfactant (Phosphanol RL-210, manufactured by tokyo chemical industries co., ltd.) as a binder was prepared.
The adhesive solution was applied to one surface of a substrate (multilayer polyolefin film, thickness: 100 μm), and then dried at 70 ℃ for 60 seconds to form an adhesive layer having a thickness of 10 μm, thereby obtaining an adhesive sheet.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
[ example 2]
A pressure-sensitive adhesive sheet was obtained in the same manner as in example 1 except that AN acrylic copolymer (butyl acrylate (BA)/Acrylonitrile (AN)/hydroxyethyl acrylate (HEA) (weight ratio) 72/27/5, weight average molecular weight: 960000) was used instead of the acrylic copolymer (butyl acrylate (BA)/Acrylonitrile (AN)/Acrylic Acid (AA) (weight ratio) 72/27/1, weight average molecular weight: 800000).
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
[ example 3]
A pressure-sensitive adhesive sheet was obtained in the same manner as in example 1 except that AN acrylic copolymer (butyl acrylate (BA)/methacrylic acid (MMA)/hydroxyethyl acrylate (HEA) (weight ratio) 64/33/3, weight average molecular weight: 500000) was used instead of the acrylic copolymer (butyl acrylate (BA)/Acrylonitrile (AN)/Acrylic Acid (AA) (weight ratio) 72/27/1, weight average molecular weight: 800000).
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
[ example 4]
A pressure-sensitive adhesive sheet was obtained in the same manner as in example 1 except that AN acrylic copolymer (butyl acrylate (BA)/methacrylic acid (MMA)/hydroxyethyl acrylate (HEA) (weight ratio) 56/41/3, weight average molecular weight: 440000) was used instead of the acrylic copolymer (butyl acrylate (BA)/Acrylonitrile (AN)/Acrylic Acid (AA) (weight ratio) 72/27/1, weight average molecular weight: 800000).
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
[ example 5]
An ethyl acetate solution containing 100 parts by weight of an acrylic copolymer (butyl acrylate (BA)/methacrylic acid (MMA)/hydroxyethyl acrylate (HEA) (weight ratio) 56/41/3, weight average molecular weight: 440000), 0.25 parts by weight of ethylenediamine polyol (ADEKA EDP-300, manufactured by ADEKA corporation), 0.50 parts by weight of an isocyanate crosslinking agent (Coronate L, manufactured by tokyo co., ltd.), and 0.5 parts by weight of a phosphate surfactant (Phosphanol RL-210, manufactured by tokyo chemical industries co., ltd.) was prepared.
The adhesive solution was applied to one surface of a substrate (multilayer polyolefin film, thickness: 80 μm), and then dried at 70 ℃ for 60 seconds to form an adhesive layer having a thickness of 10 μm, thereby obtaining an adhesive sheet.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
[ example 6]
A pressure-sensitive adhesive sheet was obtained in the same manner as in example 1 except that AN acrylic copolymer (butyl acrylate (BA)/methacrylic acid (MMA)/hydroxyethyl acrylate (HEA) (weight ratio) of 48.5/48.5/3 and weight-average molecular weight: 430000) was used instead of the acrylic copolymer (butyl acrylate (BA)/Acrylonitrile (AN)/Acrylic Acid (AA) (weight ratio) of 72/27/1 and weight-average molecular weight: 800000).
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
[ example 7]
AN ethyl acetate solution containing 100 parts by weight of AN acrylic copolymer (weight average molecular weight: 800000)) composed of Butyl Acrylate (BA)/Acrylonitrile (AN)/Acrylic Acid (AA) (weight ratio): 72/27/1, 0.25 parts by weight of ethylenediamine polyol (ADEKA EDP-300, manufactured by ADEKA corporation), 0.50 parts by weight of AN isocyanate-based crosslinking agent (Coronate L, manufactured by tokyo co., ltd.), and 0.5 parts by weight of a phosphate-based surfactant (Phosphanol RL-210, manufactured by tokyo chemical co., ltd.) was prepared.
The adhesive solution was applied to one surface of a substrate (polyethylene film, thickness: 100 μm), and then dried at 70 ℃ for 60 seconds to form an adhesive layer having a thickness of 10 μm, thereby obtaining an adhesive sheet.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
[ example 8]
AN ethyl acetate solution containing 100 parts by weight of AN acrylic copolymer (weight average molecular weight: 800000)) composed of Butyl Acrylate (BA)/Acrylonitrile (AN)/Acrylic Acid (AA) (weight ratio): 72/27/1, 0.25 parts by weight of ethylenediamine polyol (ADEKA EDP-300, manufactured by ADEKA corporation), 0.50 parts by weight of AN isocyanate-based crosslinking agent (Coronate L, manufactured by tokyo co., ltd.), and 0.5 parts by weight of a phosphate-based surfactant (Phosphanol RL-210, manufactured by tokyo chemical co., ltd.) was prepared.
The adhesive solution was applied to one surface of a substrate (special polyolefin film, thickness: 80 μm), and then dried at 70 ℃ for 60 seconds to form an adhesive layer having a thickness of 10 μm, thereby obtaining an adhesive sheet.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
[ example 9]
A psa sheet was obtained in the same manner as in example 6, except that the thickness of the psa layer was 20 μm.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
[ example 10]
An ethyl acetate solution containing 100 parts by weight of an acrylic copolymer (butyl acrylate (BA)/methacrylic acid (MMA)/hydroxyethyl acrylate (HEA) (weight ratio): 48.5/48.5/3, weight average molecular weight: 430000), 0.25 parts by weight of ethylenediamine polyol (ADEKA Polyether EDP-300, manufactured by ADEKA corporation), 0.50 parts by weight of an isocyanate crosslinking agent (Coronate L, manufactured by tokyo co., ltd.), and 0.5 parts by weight of a phosphate surfactant (Phosphanol RL-210, manufactured by tokyo chemical industries co., ltd.) as an adhesive was prepared.
The pressure-sensitive adhesive solution was applied to the release-treated surface of a release liner coated with an Si release agent, and then dried at 70 ℃ for 120 seconds to obtain a substrate-less pressure-sensitive adhesive sheet having a thickness of 100 μm.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
[ example 11]
An ethyl acetate solution containing 100 parts by weight of an acrylic copolymer ((butyl acrylate (BA)/methacrylic acid (MMA)/Acrylic Acid (AA) (weight ratio) ═ 52/45/1, weight average molecular weight: 550000), 0.25 parts by weight of ethylenediamine polyol (ADEKA Polyether EDP-300, manufactured by ADEKA corporation), 0.50 parts by weight of an isocyanate-based crosslinking agent (Coronate L, manufactured by tokyo co., ltd.), and 0.1 parts by weight of a phosphate-based surfactant (Phosphanol RL-210, manufactured by tokyo chemical industries, ltd.) was prepared.
The adhesive solution was applied to one surface of a substrate (multilayer polyolefin film, thickness: 100 μm), and then dried at 70 ℃ for 60 seconds to form an adhesive layer having a thickness of 10 μm, thereby obtaining an adhesive sheet.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
[ example 12]
An ethyl acetate solution containing 100 parts by weight of an acrylic copolymer ((butyl acrylate (BA)/methacrylic acid (MMA)/Acrylic Acid (AA) (weight ratio): 48.5/48.5/1, weight average molecular weight: 550000), 0.25 parts by weight of ethylenediamine polyol (ADEKA EDP-300, manufactured by ADEKA corporation), 0.50 parts by weight of an isocyanate-based crosslinking agent (Coronate L, manufactured by tokyo co., ltd.), and 0.1 parts by weight of a phosphate-based surfactant (Phosphanol RL-210, manufactured by tokyo chemical industries, ltd.) as an adhesive was prepared.
The adhesive solution was applied to one surface of a substrate (multilayer polyolefin film, thickness: 100 μm), and then dried at 70 ℃ for 60 seconds to form an adhesive layer having a thickness of 10 μm, thereby obtaining an adhesive sheet.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
Comparative example 1
AN ethyl acetate solution containing 100 parts by weight of AN acrylic copolymer (weight average molecular weight: 800000)) composed of Butyl Acrylate (BA)/Acrylonitrile (AN)/Acrylic Acid (AA) (weight ratio): 85/15/2.5, 0.25 parts by weight of ethylenediamine polyol (ADEKA Polyether EDP-300, manufactured by ADEKA corporation), 0.50 parts by weight of AN isocyanate crosslinking agent (Coronate L, manufactured by tokyo co., ltd.), and 0.5 parts by weight of a phosphate surfactant (Phosphanol RL-210, manufactured by tokyo chemical industries, ltd.) as a binder was prepared.
The adhesive solution was applied to one surface of a substrate (multilayer polyolefin film, thickness: 100 μm), and then dried at 70 ℃ for 60 seconds to form an adhesive layer having a thickness of 10 μm, thereby obtaining an adhesive sheet.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
Comparative example 2
A pressure-sensitive adhesive sheet was obtained in the same manner as in comparative example 1, except that AN acrylic copolymer (butyl acrylate (BA)/Acrylonitrile (AN)/Acrylic Acid (AA) (weight ratio) of 100/5, weight average molecular weight: 800000) was used instead of the acrylic copolymer (butyl acrylate (BA)/Acrylonitrile (AN)/Acrylic Acid (AA) (weight ratio) of 85/15/2.5, weight average molecular weight: 800000).
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
Comparative example 3
An ethyl acetate solution containing 100 parts by weight of an acrylic copolymer (weight average molecular weight: 550000) composed of 2-ethylhexyl acrylate (2 EHA)/hydroxyethyl acrylate (HEA) (weight ratio): 100/3), 0.25 parts by weight of ethylenediamine polyol (ADEKA Polyether EDP-300, manufactured by ADEKA corporation), 0.50 parts by weight of an isocyanate crosslinking agent (Coronate L, manufactured by tokyo co., ltd.) and 0.5 parts by weight of a phosphate surfactant (Phosphanol RL-210, manufactured by tokyo chemical industries co., ltd.) was prepared.
The adhesive solution was applied to one surface of a substrate (polyethylene film, thickness: 60 μm), and then dried at 70 ℃ for 60 seconds to form an adhesive layer having a thickness of 10 μm, thereby obtaining an adhesive sheet.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
Comparative example 4
AN ethyl acetate solution containing 100 parts by weight of AN acrylic copolymer (weight average molecular weight: 800000)) composed of Butyl Acrylate (BA)/Acrylonitrile (AN)/Acrylic Acid (AA) (weight ratio): 72/27/1, 0.25 parts by weight of ethylenediamine polyol (ADEKA EDP-300, manufactured by ADEKA corporation), 0.50 parts by weight of AN isocyanate-based crosslinking agent (Coronate L, manufactured by tokyo co., ltd.), 2.00 parts by weight of AN epoxy-based crosslinking agent (TETRAD-C, manufactured by mitsubishi gas chemical corporation), and 0.5 parts by weight of a phosphate-based surfactant (Phosphanol RL-210, manufactured by tokyo chemical industry co., ltd.) was prepared.
The adhesive solution was applied to one surface of a substrate (multilayer polyolefin film, thickness: 100 μm), and then dried at 70 ℃ for 60 seconds to form an adhesive layer having a thickness of 10 μm, thereby obtaining an adhesive sheet.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
Comparative example 5
An ethyl acetate solution containing 100 parts by weight of a double bond-introduced acrylic copolymer (acrylic copolymer comprising alkyl methacrylate/2-hydroxyethyl methacrylate/Karenz MOI (weight ratio) 90.71/9.29/9.07 (weight average molecular weight 500000)), 3 parts by weight of polypropylene glycol (Polyhardener D-100, manufactured by first industrial pharmaceutical co., ltd.), 2 parts by weight of an isocyanate-based crosslinking agent (Coronate L, manufactured by tokyo co., ltd.), and 3 parts by weight of a binder (Irgacure 184, manufactured by IGM Resins lia s.r.l.) was prepared.
The adhesive solution was applied to one surface of a substrate (multilayer polyolefin film, thickness: 80 μm), and then dried at 70 ℃ for 60 seconds to form an adhesive layer having a thickness of 8 μm, thereby obtaining an adhesive sheet.
The obtained pressure-sensitive adhesive sheets were subjected to the above evaluations (1) to (6), and the results are shown in table 1.
As is clear from table 1, the pressure-sensitive adhesive sheet of the present invention has appropriate adhesive strength, excellent peelability, and excellent concave-convex following properties.
Claims (8)
1. An adhesive sheet comprising an adhesive layer, wherein,
when the pressure-sensitive adhesive layer of the pressure-sensitive adhesive sheet is adhered to a Polyimide (PI) film, the adhesive strength at 23 ℃ is 2N/20mm or less,
the adhesive layer has an indentation hardness of 3MPa or less at 70 ℃.
2. The adhesive sheet according to claim 1, wherein,
the adhesive layer has an indentation modulus at 25 ℃ of 25MPa or more.
3. The adhesive sheet according to claim 1 or 2,
the adhesive layer comprises an acrylic adhesive comprising an acrylic polymer as a base polymer,
the glass transition temperature of the acrylic polymer is-35 ℃ or higher.
4. The adhesive sheet according to any one of claims 1 to 3,
the adhesive layer has a gel fraction of 70% or less.
5. The adhesive sheet according to any one of claims 1 to 4,
the thickness of the adhesive layer is 2-200 μm.
6. The adhesive sheet according to any one of claims 1 to 5, further comprising a substrate, the adhesive layer being disposed on at least one side of the substrate.
7. The adhesive sheet according to claim 6, which has a storage modulus E' at 70 ℃ of 6X 107Pa or less.
8. The adhesive sheet according to claim 6 or 7,
the thickness of the base material is 30-150 mu m.
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| JP2020075987 | 2020-04-22 | ||
| JP2020-075987 | 2020-04-22 | ||
| JP2021-031655 | 2021-03-01 | ||
| JP2021031655A JP2021175789A (en) | 2020-04-22 | 2021-03-01 | Adhesive sheet |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013163775A (en) * | 2012-02-13 | 2013-08-22 | Nitto Denko Corp | Adhesive tape |
| CN107641484A (en) * | 2016-07-22 | 2018-01-30 | 三星电子株式会社 | Adhesive, the method for preparing the adhesive and electrode and lithium battery including the adhesive |
| WO2020049986A1 (en) * | 2018-09-06 | 2020-03-12 | 日東電工株式会社 | Adhesive sheet |
-
2021
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- 2021-04-21 CN CN202110428849.9A patent/CN113528033A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013163775A (en) * | 2012-02-13 | 2013-08-22 | Nitto Denko Corp | Adhesive tape |
| CN107641484A (en) * | 2016-07-22 | 2018-01-30 | 三星电子株式会社 | Adhesive, the method for preparing the adhesive and electrode and lithium battery including the adhesive |
| WO2020049986A1 (en) * | 2018-09-06 | 2020-03-12 | 日東電工株式会社 | Adhesive sheet |
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