JP5686543B2 - Adhesive and adhesive sheet using the same - Google Patents
Adhesive and adhesive sheet using the same Download PDFInfo
- Publication number
- JP5686543B2 JP5686543B2 JP2010162308A JP2010162308A JP5686543B2 JP 5686543 B2 JP5686543 B2 JP 5686543B2 JP 2010162308 A JP2010162308 A JP 2010162308A JP 2010162308 A JP2010162308 A JP 2010162308A JP 5686543 B2 JP5686543 B2 JP 5686543B2
- Authority
- JP
- Japan
- Prior art keywords
- component
- pressure
- sensitive adhesive
- meth
- adhesive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000853 adhesive Substances 0.000 title claims description 75
- 230000001070 adhesive effect Effects 0.000 title claims description 75
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims description 87
- 239000004925 Acrylic resin Substances 0.000 claims description 32
- 229920000178 Acrylic resin Polymers 0.000 claims description 32
- 239000000945 filler Substances 0.000 claims description 23
- 239000002253 acid Substances 0.000 claims description 22
- 125000000524 functional group Chemical group 0.000 claims description 19
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 19
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 17
- 239000003431 cross linking reagent Substances 0.000 claims description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- -1 acryl Chemical group 0.000 description 28
- 230000009477 glass transition Effects 0.000 description 26
- 239000010410 layer Substances 0.000 description 23
- 239000000178 monomer Substances 0.000 description 22
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 21
- 239000003063 flame retardant Substances 0.000 description 21
- 238000000576 coating method Methods 0.000 description 20
- 239000002245 particle Substances 0.000 description 20
- 239000011248 coating agent Substances 0.000 description 19
- 239000010408 film Substances 0.000 description 19
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 17
- 239000006258 conductive agent Substances 0.000 description 17
- 230000007423 decrease Effects 0.000 description 16
- 239000000470 constituent Substances 0.000 description 14
- 238000004132 cross linking Methods 0.000 description 14
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 12
- 239000004593 Epoxy Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 239000012790 adhesive layer Substances 0.000 description 10
- 239000000758 substrate Substances 0.000 description 10
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 8
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 229920000139 polyethylene terephthalate Polymers 0.000 description 7
- 239000005020 polyethylene terephthalate Substances 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 6
- 125000003700 epoxy group Chemical group 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229920001296 polysiloxane Polymers 0.000 description 6
- 150000003839 salts Chemical group 0.000 description 6
- 125000000217 alkyl group Chemical group 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 125000003368 amide group Chemical group 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000004088 foaming agent Substances 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 239000003381 stabilizer Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000007334 copolymerization reaction Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 239000012948 isocyanate Substances 0.000 description 3
- 150000002513 isocyanates Chemical class 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 125000000542 sulfonic acid group Chemical group 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004604 Blowing Agent Substances 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 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
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 108010039918 Polylysine Chemical class 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- ZOJBYZNEUISWFT-UHFFFAOYSA-N allyl isothiocyanate Chemical compound C=CCN=C=S ZOJBYZNEUISWFT-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 229960000686 benzalkonium chloride Drugs 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 208000028659 discharge Diseases 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000656 polylysine Chemical class 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 235000007586 terpenes Nutrition 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 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
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- POTYORUTRLSAGZ-UHFFFAOYSA-N (3-chloro-2-hydroxypropyl) prop-2-enoate Chemical compound ClCC(O)COC(=O)C=C POTYORUTRLSAGZ-UHFFFAOYSA-N 0.000 description 1
- 125000004400 (C1-C12) alkyl group Chemical group 0.000 description 1
- XXANGWUMCMNLJD-UHFFFAOYSA-N 1-(benzenesulfonamido)-3-(benzenesulfonamidocarbamoylamino)oxyurea Chemical compound C=1C=CC=CC=1S(=O)(=O)NNC(=O)NONC(=O)NNS(=O)(=O)C1=CC=CC=C1 XXANGWUMCMNLJD-UHFFFAOYSA-N 0.000 description 1
- SDXHBDVTZNMBEW-UHFFFAOYSA-N 1-ethoxy-2-(2-hydroxyethoxy)ethanol Chemical compound CCOC(O)COCCO SDXHBDVTZNMBEW-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- RXGSAYBOEDPICZ-UHFFFAOYSA-N 2-[6-[[amino-(diaminomethylideneamino)methylidene]amino]hexyl]-1-(diaminomethylidene)guanidine Chemical compound NC(N)=NC(N)=NCCCCCCN=C(N)N=C(N)N RXGSAYBOEDPICZ-UHFFFAOYSA-N 0.000 description 1
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- YZTJKOLMWJNVFH-UHFFFAOYSA-N 2-sulfobenzene-1,3-dicarboxylic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1S(O)(=O)=O YZTJKOLMWJNVFH-UHFFFAOYSA-N 0.000 description 1
- BLJHFERYMGMXSC-UHFFFAOYSA-N 3-[3-(hydrazinesulfonyl)phenyl]sulfonylbenzenesulfonohydrazide Chemical compound NNS(=O)(=O)C1=CC=CC(S(=O)(=O)C=2C=C(C=CC=2)S(=O)(=O)NN)=C1 BLJHFERYMGMXSC-UHFFFAOYSA-N 0.000 description 1
- QOXOZONBQWIKDA-UHFFFAOYSA-N 3-hydroxypropyl Chemical group [CH2]CCO QOXOZONBQWIKDA-UHFFFAOYSA-N 0.000 description 1
- NBOCQTNZUPTTEI-UHFFFAOYSA-N 4-[4-(hydrazinesulfonyl)phenoxy]benzenesulfonohydrazide Chemical compound C1=CC(S(=O)(=O)NN)=CC=C1OC1=CC=C(S(=O)(=O)NN)C=C1 NBOCQTNZUPTTEI-UHFFFAOYSA-N 0.000 description 1
- NSXHGNRQESFGHM-UHFFFAOYSA-N 4-ethenyl-n,n-dimethylbenzenesulfonamide Chemical compound CN(C)S(=O)(=O)C1=CC=C(C=C)C=C1 NSXHGNRQESFGHM-UHFFFAOYSA-N 0.000 description 1
- SXIFAEWFOJETOA-UHFFFAOYSA-N 4-hydroxy-butyl Chemical group [CH2]CCCO SXIFAEWFOJETOA-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical group NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 1
- 239000004156 Azodicarbonamide Substances 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- XNCOSPRUTUOJCJ-UHFFFAOYSA-N Biguanide Chemical group NC(N)=NC(N)=N XNCOSPRUTUOJCJ-UHFFFAOYSA-N 0.000 description 1
- 229940123208 Biguanide Drugs 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 239000004287 Dehydroacetic acid Substances 0.000 description 1
- MWRWFPQBGSZWNV-UHFFFAOYSA-N Dinitrosopentamethylenetetramine Chemical compound C1N2CN(N=O)CN1CN(N=O)C2 MWRWFPQBGSZWNV-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 150000004008 N-nitroso compounds Chemical class 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
- TUEIURIZJQRMQE-UHFFFAOYSA-N [2-(tert-butylsulfamoyl)phenyl]boronic acid Chemical compound CC(C)(C)NS(=O)(=O)C1=CC=CC=C1B(O)O TUEIURIZJQRMQE-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 235000016720 allyl isothiocyanate Nutrition 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- CAMXVZOXBADHNJ-UHFFFAOYSA-N ammonium nitrite Chemical compound [NH4+].[O-]N=O CAMXVZOXBADHNJ-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 150000001540 azides Chemical class 0.000 description 1
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 description 1
- 235000019399 azodicarbonamide Nutrition 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 150000001558 benzoic acid derivatives Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000012662 bulk polymerization Methods 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- FAOSYNUKPVJLNZ-UHFFFAOYSA-N butylstannane Chemical compound CCCC[SnH3] FAOSYNUKPVJLNZ-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- IQBJFLXHQFMQRP-UHFFFAOYSA-K calcium;zinc;phosphate Chemical compound [Ca+2].[Zn+2].[O-]P([O-])([O-])=O IQBJFLXHQFMQRP-UHFFFAOYSA-K 0.000 description 1
- VPKDCDLSJZCGKE-UHFFFAOYSA-N carbodiimide group Chemical group N=C=N VPKDCDLSJZCGKE-UHFFFAOYSA-N 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- CZRDZAGTSCUWNG-UHFFFAOYSA-M chloro(dimethyl)tin Chemical compound C[Sn](C)Cl CZRDZAGTSCUWNG-UHFFFAOYSA-M 0.000 description 1
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 description 1
- 229940018557 citraconic acid Drugs 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 125000002704 decyl 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])* 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000019258 dehydroacetic acid Nutrition 0.000 description 1
- JEQRBTDTEKWZBW-UHFFFAOYSA-N dehydroacetic acid Chemical compound CC(=O)C1=C(O)OC(C)=CC1=O JEQRBTDTEKWZBW-UHFFFAOYSA-N 0.000 description 1
- 229940061632 dehydroacetic acid Drugs 0.000 description 1
- PGRHXDWITVMQBC-UHFFFAOYSA-N dehydroacetic acid Natural products CC(=O)C1C(=O)OC(C)=CC1=O PGRHXDWITVMQBC-UHFFFAOYSA-N 0.000 description 1
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- UMNKXPULIDJLSU-UHFFFAOYSA-N dichlorofluoromethane Chemical compound FC(Cl)Cl UMNKXPULIDJLSU-UHFFFAOYSA-N 0.000 description 1
- 229940099364 dichlorofluoromethane Drugs 0.000 description 1
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 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 1
- 239000000975 dye Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000004049 embossing Methods 0.000 description 1
- 238000010556 emulsion polymerization method Methods 0.000 description 1
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- 150000002366 halogen compounds Chemical class 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 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 1
- 238000007602 hot air drying Methods 0.000 description 1
- 150000002429 hydrazines Chemical class 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-IHWYPQMZSA-N isocrotonic acid Chemical compound C\C=C/C(O)=O LDHQCZJRKDOVOX-IHWYPQMZSA-N 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- HNEGQIOMVPPMNR-NSCUHMNNSA-N mesaconic acid Chemical compound OC(=O)C(/C)=C/C(O)=O HNEGQIOMVPPMNR-NSCUHMNNSA-N 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- HNEGQIOMVPPMNR-UHFFFAOYSA-N methylfumaric acid Natural products OC(=O)C(C)=CC(O)=O HNEGQIOMVPPMNR-UHFFFAOYSA-N 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- GEMHFKXPOCTAIP-UHFFFAOYSA-N n,n-dimethyl-n'-phenylcarbamimidoyl chloride Chemical compound CN(C)C(Cl)=NC1=CC=CC=C1 GEMHFKXPOCTAIP-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 125000002347 octyl 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])[H] 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 239000002530 phenolic antioxidant Substances 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000223 polyglycerol Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002683 reaction inhibitor Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 150000003873 salicylate salts Chemical class 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- DUIOPKIIICUYRZ-UHFFFAOYSA-N semicarbazide Chemical compound NNC(N)=O DUIOPKIIICUYRZ-UHFFFAOYSA-N 0.000 description 1
- 150000003349 semicarbazides Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000004334 sorbic acid Substances 0.000 description 1
- 235000010199 sorbic acid Nutrition 0.000 description 1
- 229940075582 sorbic acid Drugs 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 1
- 238000010558 suspension polymerization method Methods 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 125000002298 terpene group Chemical group 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- AFCAKJKUYFLYFK-UHFFFAOYSA-N tetrabutyltin Chemical compound CCCC[Sn](CCCC)(CCCC)CCCC AFCAKJKUYFLYFK-UHFFFAOYSA-N 0.000 description 1
- YGNGABUJMXJPIJ-UHFFFAOYSA-N thiatriazole Chemical compound C1=NN=NS1 YGNGABUJMXJPIJ-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 125000005208 trialkylammonium group Chemical group 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- CYRMSUTZVYGINF-UHFFFAOYSA-N trichlorofluoromethane Chemical compound FC(Cl)(Cl)Cl CYRMSUTZVYGINF-UHFFFAOYSA-N 0.000 description 1
- 229940029284 trichlorofluoromethane Drugs 0.000 description 1
- SOLUNJPVPZJLOM-UHFFFAOYSA-N trizinc;distiborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-][Sb]([O-])([O-])=O.[O-][Sb]([O-])([O-])=O SOLUNJPVPZJLOM-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Description
本発明は、粘着剤及びこれを用いた粘着シートに関する。具体的には、熱伝導剤、難燃剤、発泡剤、導電剤といったフィラーを粘着剤層中に高充填した粘着剤及び粘着シートに関する。 The present invention relates to a pressure-sensitive adhesive and a pressure-sensitive adhesive sheet using the same. Specifically, the present invention relates to a pressure-sensitive adhesive and a pressure-sensitive adhesive sheet in which a pressure-sensitive adhesive layer is highly filled with a filler such as a heat conductive agent, a flame retardant, a foaming agent, and a conductive agent.
粘着剤に求められる基本特性として、粘着力、タック、保持力の3つの特性を挙げることができるが、これらをバランスよく調整することができる点から、アクリル系粘着剤の開発が盛んに行われている。電子機器の高機能化を図るため、その部材である粘着シートに対しても高機能化が求められており、これを実現するための一つの手段として、熱伝導剤、難燃剤、導電剤等のフィラーを粘着剤中に多量に配合させる方法が提案されている（例えば特許文献１〜３参照）。これらのものは粘着力を維持するためには熱伝導剤、難燃剤等の配合量を増やすことができず、熱伝導性、難燃性等の効果がいまだ不十分なものであった。 There are three basic properties required for adhesives: adhesive strength, tack, and holding power. Acrylic adhesives have been actively developed because they can be balanced. ing. In order to increase the functionality of electronic equipment, the adhesive sheet as a member is also required to have higher functionality, and as one means for realizing this, a thermal conductive agent, a flame retardant, a conductive agent, etc. There has been proposed a method of blending a large amount of the above filler into the pressure-sensitive adhesive (see, for example, Patent Documents 1 to 3). In order to maintain the adhesive strength, these compounds cannot increase the blending amount of a heat conductive agent, a flame retardant and the like, and effects such as heat conductivity and flame retardancy are still insufficient.
本発明は、上記した従来の粘着剤及び粘着シートが有する欠点を克服し、柔軟性及び粘着性の何れの特性を維持しつつフィラーを高充填可能な粘着剤及びこれを利用した粘着シートを提供するためになされたものである。 The present invention provides a pressure-sensitive adhesive that can overcome the drawbacks of the above-mentioned conventional pressure-sensitive adhesives and pressure-sensitive adhesive sheets and can be highly filled with a filler while maintaining any of the properties of flexibility and pressure-sensitive adhesive, and a pressure-sensitive adhesive sheet using the same. It was made to do.
本発明者らは、粘着剤にフィラーを高充填させた場合においても、柔軟性と粘着性を同時に満足するためには、活性水素含有基を有し、所定の分子量からなる（メタ）アクリル系樹脂及び特定の（メタ）アクリル系架橋剤からなる粘着剤及びこれを用いた粘着シートであることが必要であることを見出し、この知見に基づいて本発明をなすに至った。 The present inventors have a (meth) acrylic group having an active hydrogen-containing group and having a predetermined molecular weight in order to satisfy flexibility and adhesiveness at the same time even when the adhesive is highly filled with a filler. The present inventors have found that it is necessary to be a pressure-sensitive adhesive composed of a resin and a specific (meth) acrylic crosslinking agent and a pressure-sensitive adhesive sheet using the same, and have come to make the present invention based on this finding.
すなわち、本発明は以下の粘着剤及び粘着シートを提供するものである。 That is, the present invention provides the following pressure-sensitive adhesive and pressure-sensitive adhesive sheet.
［１］（Ａ）活性水素含有基を有し、質量平均分子量が８００〜２０，０００の範囲である（メタ）アクリル系樹脂と（Ｂ）前記（Ａ）成分と架橋する官能基を有し、その官能基の官能基当量が２００〜１５００ｇ／ｅｑの範囲である（メタ）アクリル系架橋剤及び（Ｄ）フィラ―からなる粘着剤であって、前記（Ｄ）成分の粘着剤中の配合割合が５０体積％〜８０体積％の範囲であることを特徴とする粘着剤。 [ 1 ] (A) It has an active hydrogen-containing group and has a (meth) acrylic resin having a mass average molecular weight in the range of 800 to 20,000 and (B) a functional group that crosslinks with the component (A). , A pressure-sensitive adhesive comprising a (meth) acrylic crosslinking agent having a functional group equivalent weight of 200 to 1500 g / eq and (D) filler, wherein the component (D) is contained in the pressure-sensitive adhesive. A pressure-sensitive adhesive having a ratio in the range of 50% by volume to 80% by volume.
［２］更に、（Ｃ）活性水素含有基を有し、質量平均分子量が２０万〜２００万の範囲である（メタ）アクリル系樹脂を含有することを特徴とする［１］に記載の粘着剤。 [2] The adhesive according to [1], further comprising (C) a (meth) acrylic resin having an active hydrogen-containing group and a mass average molecular weight in the range of 200,000 to 2,000,000. Agent.
［３］（Ａ）成分の酸価が２５〜１５０ｍｇＫＯＨ／ｇ、（Ｃ）成分の酸価が３〜２０ｍｇＫＯＨ／ｇであることを特徴とする［２］に記載の粘着剤。 [3] The pressure-sensitive adhesive according to [2], wherein the acid value of the component (A) is 25 to 150 mgKOH / g, and the acid value of the component (C) is 3 to 20 mgKOH / g.
［４］（Ａ）成分の水酸基価が２５〜１５０ｍｇＫＯＨ／ｇ、（Ｃ）成分の水酸基価が３〜２０ｍｇＫＯＨ／ｇであることを特徴とする［２］に記載の粘着剤。 [4] The pressure-sensitive adhesive according to [2], wherein the component (A) has a hydroxyl value of 25 to 150 mgKOH / g, and the component (C) has a hydroxyl value of 3 to 20 mgKOH / g.
［５］［１］〜［４］何れかに記載の粘着剤をシート状若しくはフイルム上に成形した粘着シート。 [ 5 ] A pressure-sensitive adhesive sheet obtained by molding the pressure-sensitive adhesive according to any one of [1] to [ 4 ] on a sheet or film.
［６］ＪＩＳ Ｐ８１１３に準拠して測定した引張破断伸びが３０％以上であることを特徴とする［５］に記載の粘着シート。 [ 6 ] The adhesive sheet according to [ 5 ], wherein the tensile elongation at break measured in accordance with JIS P8113 is 30% or more.
本発明によれば、粘着剤中にフィラーを多量に配合することが可能であるという特徴を有するため、この粘着剤をシート状に形成したものは、使用するフィラーの性能を向上させ、かつ、柔軟性や粘着性を損なうことがない粘着シートとすることができる。例えば、フィラーとして熱伝導剤を使用した場合にはＩＣパッケージ、トランジスタ若しくはダイオード等の電子部品又は、プラズマディスプレイパネル若しくは液晶ディスプレイパネル等のパネル自体から発生した熱をヒートシンクや放熱金属板等の放熱体に効率よく伝達させるために使用し得る高熱伝導粘着シートを得ることができる。また、フィラーを多量に配合することができるため、複合機能を有する粘着シートも容易に得ることができる。 According to the present invention, since it has a feature that it is possible to mix a large amount of filler in the pressure-sensitive adhesive, what formed this pressure-sensitive adhesive in a sheet shape improves the performance of the filler used, and It can be set as the adhesive sheet which does not impair a softness | flexibility and adhesiveness. For example, when a heat conductive agent is used as a filler, heat generated from an electronic component such as an IC package, a transistor or a diode, or a panel itself such as a plasma display panel or a liquid crystal display panel is used as a heat sink or a heat radiating metal plate. It is possible to obtain a high thermal conductive pressure-sensitive adhesive sheet that can be used for efficient transmission. Moreover, since a filler can be mix | blended in large quantities, the adhesive sheet which has a composite function can also be obtained easily.
以下、本発明の粘着剤及びこれを用いた粘着シートの形態について具体的に説明するが、本発明は以下の形態に限定されるものではなく、本発明の趣旨を逸脱しない範囲で、当業者の通常の知識に基づいて、以下の実施の形態に対し、適宜変更、改良等が加えられたものも本発明の範囲のものである。 Hereinafter, the pressure-sensitive adhesive of the present invention and the form of a pressure-sensitive adhesive sheet using the same will be specifically described. However, the present invention is not limited to the following forms, and those skilled in the art can depart from the scope of the present invention. Based on this general knowledge, the scope of the present invention also includes modifications and improvements as appropriate to the following embodiments.
［粘着剤］
［Ａ成分］
本発明で使用される（Ａ）成分は、活性水素含有基を有し、かつ、質量平均分子量が８００〜２０，０００である（メタ）アクリル系樹脂である。（Ａ）成分は、（Ｄ）成分表面との濡れ性を向上させ、（Ｄ）成分の表面処理を行うことなく（Ａ）成分と（Ｄ）成分の親和性を高めるという効果を有する。（Ａ）成分の質量平均分子量が８００未満である場合には、（Ｂ）成分と架橋した場合においても分子量がいまだ低く凝集力を確保することができず、また（Ｂ）成分の添加量等を変化させ高架橋化した場合には柔軟性を維持することが難しくなる。質量平均分子量が２０，０００を超えた場合には、（Ｄ）成分の間隙に効率的に入り込むことが難しくなる。
尚、本明細書において、「（メタ）アクリル」とは、「アクリル又はメタクリル」を意味する。活性水素含有基としては、例えば、カルボキシル基、水酸基、アミド基、アミノ基、チオール基、シアノ基、スルホン酸基、リン酸基、第４級アンモニウム（塩）基等を挙げられる。尚、これらは単独で用いてもよいし、２種以上を組み合わせて用いてもよい。
[Adhesive]
[Component A]
The component (A) used in the present invention is a (meth) acrylic resin having an active hydrogen-containing group and a mass average molecular weight of 800 to 20,000. The component (A) has an effect of improving the wettability with the surface of the component (D) and increasing the affinity between the component (A) and the component (D) without performing the surface treatment of the component (D). When the mass average molecular weight of the component (A) is less than 800, the molecular weight is still low even when crosslinked with the component (B), and the cohesive force cannot be secured, and the addition amount of the component (B), etc. It is difficult to maintain flexibility when the structure is changed to be highly crosslinked. When the mass average molecular weight exceeds 20,000, it is difficult to efficiently enter the gap of the component (D).
In the present specification, “(meth) acryl” means “acryl or methacryl”. Examples of the active hydrogen-containing group include a carboxyl group, a hydroxyl group, an amide group, an amino group, a thiol group, a cyano group, a sulfonic acid group, a phosphoric acid group, and a quaternary ammonium (salt) group. In addition, these may be used independently and may be used in combination of 2 or more type.
カルボキシル基としては、アクリル酸、メタクリル酸、イタコン酸、クロトン酸、イソクロトン酸、マレイン酸、フマル酸、シトラコン酸、メサコン酸又はこれらの単量体から誘導される官能性単量体等が挙げられる。尚、これらは単独で用いてもよいし、２種以上を組み合わせて用いてもよい。 Examples of the carboxyl group include acrylic acid, methacrylic acid, itaconic acid, crotonic acid, isocrotonic acid, maleic acid, fumaric acid, citraconic acid, mesaconic acid or functional monomers derived from these monomers. . In addition, these may be used independently and may be used in combination of 2 or more type.
水酸基としては、例えば、（メタ）アクリル酸２−ヒドロキシエチル、（メタ）アクリル酸３−ヒドロキシプロピル、（メタ）アクリル酸２−ヒドロキシブチル、（メタ）アクリル酸４−ヒドロキシブチル、（メタ）アクリル酸６−ヒドロキシヘキシル、（メタ）アクリル酸８−ヒドロキシオクチル、（メタ）アクリル酸１０−ヒドロキシデシル、（メタ）アクリル酸１２−ヒドロキシラクジル、（メタ）アクリル酸４−ヒドロキシメチルシクロヘキシル、（メタ）アクリル酸３−クロロ−２−ヒドロキシプロピル、（メタ）アクリル酸エトキシジエチレングリコール、（メタ）アクリル酸カプロラクトン、（メタ）アクリル酸ポリエチレングリコール、（メタ）アクリル酸ポリプロピレングリコール等が挙げられる。尚、これらは単独で用いてもよいし、２種以上を組み合わせて用いてもよい。 Examples of the hydroxyl group include 2-hydroxyethyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, and (meth) acrylic. 6-hydroxyhexyl acid, 8-hydroxyoctyl (meth) acrylate, 10-hydroxydecyl (meth) acrylate, 12-hydroxylactyl (meth) acrylate, 4-hydroxymethylcyclohexyl (meth) acrylate, (meth ) 3-chloro-2-hydroxypropyl acrylate, ethoxydiethylene glycol (meth) acrylate, caprolactone (meth) acrylate, polyethylene glycol (meth) acrylate, polypropylene glycol (meth) acrylate, and the like. In addition, these may be used independently and may be used in combination of 2 or more type.
アミド基としては、（メタ）アクリルアミド、α−エチル（メタ）アクリルアミド、Ｎ−メチル（メタ）アクリルアミド、Ｎ−ブトキシメチル（メタ）アクリルアミド、ジアセトン（メタ）アクリルアミド、Ｎ，Ｎ−ジメチル（メタ）アクリルアミド、Ｎ，Ｎ−ジエチル（メタ）アクリルアミド、Ｎ，Ｎ−ジメチル−ｐ−スチレンスルホンアミド、Ｎ，Ｎ−ジメチルアミノエチル（メタ）アクリルアミド、Ｎ，Ｎ−ジエチルアミノエチル（メタ）アクリルアミド、Ｎ，Ｎ−ジメチルアミノプロピル（メタ）アクリルアミド、Ｎ，Ｎ−ジエチルアミノプロピル（メタ）アクリルアミド等が挙げられる。尚、これらは、単独で用いてもよいし、２種以上を組み合わせて用いいてもよい。 As the amide group, (meth) acrylamide, α-ethyl (meth) acrylamide, N-methyl (meth) acrylamide, N-butoxymethyl (meth) acrylamide, diacetone (meth) acrylamide, N, N-dimethyl (meth) acrylamide N, N-diethyl (meth) acrylamide, N, N-dimethyl-p-styrenesulfonamide, N, N-dimethylaminoethyl (meth) acrylamide, N, N-diethylaminoethyl (meth) acrylamide, N, N- Examples thereof include dimethylaminopropyl (meth) acrylamide and N, N-diethylaminopropyl (meth) acrylamide. In addition, these may be used independently and may be used in combination of 2 or more type.
本発明の（Ａ）成分は、前記活性水素含有基を有する単量体と炭素数１〜１２のアルキル基を有する（メタ）アクリル酸アルキルエステルからなる共重合体であり、その配合比を通常質量比で１０：９０〜２．５：９７．５の範囲としたものが好ましい。 The component (A) of the present invention is a copolymer comprising a monomer having the active hydrogen-containing group and a (meth) acrylic acid alkyl ester having an alkyl group having 1 to 12 carbon atoms. What was made into the range of 10: 90-2.5: 97.5 by mass ratio is preferable.
炭素数１〜１２のアルキル基を有する（メタ）アクリル酸アルキルエステルとしては、例えば（メタ）アクリル酸メチル、（メタ）アクリル酸エチル、（メタ）アクリル酸プロピル、（メタ）アクリル酸ブチル、（メタ）アクリル酸ヘキシル、（メタ）アクリル酸２−エチルヘキシル、（メタ）アクリル酸オクチル、（メタ）アクリル酸デシル、（メタ）アクリル酸ラウリル等が挙げられる。 Examples of the (meth) acrylic acid alkyl ester having an alkyl group having 1 to 12 carbon atoms include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, ( Examples include hexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, octyl (meth) acrylate, decyl (meth) acrylate, and lauryl (meth) acrylate.
本発明の（Ａ）成分は、前記活性水素含有基を有する単量体と炭素数１〜１２のアルキル基を有する（メタ）アクリル酸アルキルエステルからなる共重合体であることが好ましいが、これらに加えて任意的な他の単量体成分からなる共重合体とすることもできる。任意的な他の単量体成分としては、アクリロニトリル、アクリルアミド、スチレン、酢酸ビニル及びＮ−ビニルピロリドン等が挙げられる。その使用量は単量体全量に対して０〜３０質量％、好ましくは０〜１０質量％の範囲で用いられる。 The component (A) of the present invention is preferably a copolymer comprising a monomer having an active hydrogen-containing group and a (meth) acrylic acid alkyl ester having a C 1-12 alkyl group. In addition to the above, a copolymer comprising any other monomer component can also be used. Optional other monomer components include acrylonitrile, acrylamide, styrene, vinyl acetate and N-vinyl pyrrolidone. The amount used is 0 to 30% by mass, preferably 0 to 10% by mass, based on the total amount of monomers.
（Ａ）成分の共重合体は、上記の単量体成分をラジカル共重合させることによって得ることができる。この場合の共重合法としては、乳化重合法、溶液重合法、塊状重合法、懸濁重合法、光重合法など通常用いられている公知の共重合法の中から任意に選ぶことができる。また、（Ａ）成分のガラス転移温度としては、−７０℃〜−１０℃の範囲内であることが好ましい。ガラス転移温度が−７０℃未満であると、耐熱性が低下し、ガラス転移温度が−１０℃を超えた場合には、室温における粘着力が低下するからである。耐熱性と室温における粘着力という観点から、−６０〜−２５℃の範囲内であることが好ましい。 The copolymer of component (A) can be obtained by radical copolymerization of the above monomer components. In this case, the copolymerization method can be arbitrarily selected from conventionally used copolymerization methods such as an emulsion polymerization method, a solution polymerization method, a bulk polymerization method, a suspension polymerization method, and a photopolymerization method. Moreover, it is preferable that it is in the range of -70 degreeC--10 degreeC as glass transition temperature of (A) component. This is because when the glass transition temperature is less than -70 ° C, the heat resistance decreases, and when the glass transition temperature exceeds -10 ° C, the adhesive strength at room temperature decreases. From the viewpoint of heat resistance and adhesive strength at room temperature, it is preferably in the range of −60 to −25 ° C.
（Ａ）成分として、カルボキシル基、スルホン酸基等の酸性官能基を有する（メタ）アクリル系樹脂の場合に酸価は、１０ｍｇＫＯＨ／ｇ以上であることが好ましい。酸価が１０ｍｇＫＯＨ／ｇ未満である場合には（Ｂ）成分と十分に反応することができず凝集力が低下し被着体に対する粘着力が低下するからである。 In the case of a (meth) acrylic resin having an acidic functional group such as a carboxyl group or a sulfonic acid group as the component (A), the acid value is preferably 10 mgKOH / g or more. This is because when the acid value is less than 10 mgKOH / g, it cannot sufficiently react with the component (B), and the cohesive force is lowered and the adhesive force to the adherend is lowered.
［Ｂ成分］
本発明で使用される（Ｂ）成分は、官能基当量が２００〜１５００ｇ／ｅｑであるアクリル系架橋剤である。具体的には、エポキシ基、イソシアネート基、カルボジイミド基から選択される少なくとも一種の官能基を有するアクリル樹脂が挙げられる。官能基当量が２００未満であると得られる粘着剤の靱性、柔軟性が低下するため好ましくなく、官能基当量が１５００より大きい場合には架橋密度が低下し、凝集力、耐熱性が得られないため好ましくない。靱性、耐熱性等の観点から４００〜７５０の範囲であることが好ましい。尚、（Ｂ）成分は単独で用いてもよいし、２種以上を組み合わせて用いてもよい。
[B component]
The component (B) used in the present invention is an acrylic crosslinking agent having a functional group equivalent of 200 to 1500 g / eq. Specific examples include acrylic resins having at least one functional group selected from an epoxy group, an isocyanate group, and a carbodiimide group. If the functional group equivalent is less than 200, it is not preferable because the toughness and flexibility of the resulting pressure-sensitive adhesive are lowered. If the functional group equivalent is greater than 1500, the crosslinking density is lowered, and the cohesive force and heat resistance cannot be obtained. Therefore, it is not preferable. From the viewpoint of toughness, heat resistance and the like, it is preferably in the range of 400 to 750. In addition, (B) component may be used independently and may be used in combination of 2 or more type.
（Ｂ）成分の添加量は前記（Ａ）成分１００質量部又は（Ｃ）成分を併用している場合には（Ａ）成分と（Ｃ）成分の合計添加量１００質量部に対して０．５〜１００質量部の範囲内であることが好ましい。０．５質量部未満の場合には粘着剤の凝集力を確保することができなくなり、１００質量部を超えた場合には粘着剤層の柔軟性が低下するからである。凝集力と柔軟性との観点から５〜８０質量部の範囲であることが更に好ましい。 The amount of component (B) added is 100 parts by weight with respect to 100 parts by weight of component (A) and component (C) when 100 parts by weight of component (A) or component (C) is used in combination. It is preferably within the range of 5 to 100 parts by mass. This is because when the amount is less than 0.5 parts by mass, the cohesive force of the pressure-sensitive adhesive cannot be ensured, and when it exceeds 100 parts by mass, the flexibility of the pressure-sensitive adhesive layer decreases. The range of 5 to 80 parts by mass is more preferable from the viewpoints of cohesive strength and flexibility.
（Ｂ）成分のガラス転移温度は、−７０℃〜７０℃の範囲内であることが好ましい。ガラス転移温度が−７０℃未満であると、耐熱性が低下し、ガラス転移温度が７０℃を超えた場合には、室温における粘着力が低下するためである。 (B) It is preferable that the glass transition temperature of a component exists in the range of -70 degreeC-70 degreeC. This is because when the glass transition temperature is less than -70 ° C, the heat resistance decreases, and when the glass transition temperature exceeds 70 ° C, the adhesive strength at room temperature decreases.
（Ｂ）成分の質量平均分子量は、１０００〜２０，０００の範囲内であることが好ましい。質量平均分子量が１０００未満であると、耐熱性が低下し質量平均分子量が２０，０００を超えた場合には、室温における粘着力が低下するためである。 The mass average molecular weight of the component (B) is preferably in the range of 1000 to 20,000. This is because when the mass average molecular weight is less than 1000, the heat resistance is lowered, and when the mass average molecular weight exceeds 20,000, the adhesive strength at room temperature is lowered.
（Ｂ）成分には、本発明の目的を損なわない範囲において従来公知の他の架橋剤を併用することができる。具体的には、エポキシ系架橋剤、イソシアネート系架橋剤等が挙げられる。これらの架橋剤の配合割合は（Ｂ）成分に対し、１０質量％〜５０質量％の範囲内で配合することが好ましい。 In the component (B), other conventionally known crosslinking agents can be used in combination as long as the object of the present invention is not impaired. Specifically, an epoxy type crosslinking agent, an isocyanate type crosslinking agent, etc. are mentioned. It is preferable to mix | blend the mixture ratio of these crosslinking agents in the range of 10 mass%-50 mass% with respect to (B) component.
［Ｃ成分］
（Ａ）、（Ｂ）成分のみでも本発明の目的を達成できるものであるが、（Ｃ）成分として質量平均分子量２０万〜２００万の（メタ）アクリル系樹脂を配合することが好ましい。（Ｃ）成分を配合することにより、粘着剤に靭性を付与することができ、これからなる粘着剤を柔軟、かつ、形態安定性に優れたものとすることができるからである。（Ｃ）成分の質量平均分子量が２０万未満である場合には、粘着剤の靭性を向上させる効果に乏しく、質量平均分子量が２００万を超えた場合には、粘着剤の柔軟性が低下し、被着体に対する粘着力が低下することになるからである。
[C component]
Although only the components (A) and (B) can achieve the object of the present invention, it is preferable to blend a (meth) acrylic resin having a mass average molecular weight of 200,000 to 2,000,000 as the component (C). This is because, by blending the component (C), toughness can be imparted to the pressure-sensitive adhesive, and the pressure-sensitive adhesive comprising this can be made flexible and excellent in form stability. When the mass average molecular weight of the component (C) is less than 200,000, the effect of improving the toughness of the adhesive is poor, and when the mass average molecular weight exceeds 2 million, the flexibility of the adhesive decreases. This is because the adhesive force to the adherend is reduced.
（Ｃ）成分は先に（Ａ）成分として挙げた活性水素含有基を有する単量体、炭素数が１〜１２のアルキル基を有する（メタ）アクリル酸アルキルエステル、任意的な他のモノマー成分からなる共重合体であることが好ましい。 Component (C) is a monomer having an active hydrogen-containing group previously listed as component (A), (meth) acrylic acid alkyl ester having an alkyl group having 1 to 12 carbon atoms, and other optional monomer components A copolymer consisting of
（Ｃ）成分の共重合体は、前記（Ａ）成分と同様の方法により上記の単量体成分を重合させることによって得ることができる。また、（Ｃ）成分のガラス転移温度としては、前記（Ａ）成分と同様−７０℃〜−１０℃の範囲内であることが好ましい。ガラス転移温度が−７０℃未満であると、耐熱性が低下し、ガラス転移温度が−１０℃を超えた場合には、室温における粘着力が低下するためである。尚、（Ａ）、（Ｃ）各成分を構成する単量体中のアルキル鎖は同じものであることが好ましい。アルキル鎖が異なる場合には、相溶性が低下し均一な粘着剤を得ることが困難となるからである。 The copolymer of the component (C) can be obtained by polymerizing the monomer component by the same method as the component (A). Moreover, it is preferable that it is in the range of -70 degreeC--10 degreeC like the said (A) component as glass transition temperature of (C) component. This is because when the glass transition temperature is less than −70 ° C., the heat resistance decreases, and when the glass transition temperature exceeds −10 ° C., the adhesive strength at room temperature decreases. In addition, it is preferable that the alkyl chain in the monomer which comprises each component (A) and (C) is the same. This is because when the alkyl chains are different, the compatibility is lowered and it is difficult to obtain a uniform pressure-sensitive adhesive.
前記（Ａ）成分と（Ｃ）成分の配合比が９５：５〜３０：７０の範囲で配合することが好ましい。（Ｃ）成分の配合比が前記範囲より少ない場合には粘着剤の靭性が低下し、これからなる粘着剤層はもろくなる場合がある。また、（Ｃ）成分の配合比が前記範囲より多い場合には粘着剤層の柔軟性を確保することができず、被着体に対する接触面積が下がり、粘着力が低下するからである。 The blending ratio of the component (A) to the component (C) is preferably in the range of 95: 5 to 30:70. When the compounding ratio of the component (C) is less than the above range, the toughness of the pressure-sensitive adhesive is lowered, and the pressure-sensitive adhesive layer made of this sometimes becomes brittle. Moreover, when there are more compounding ratios of (C) component than the said range, the softness | flexibility of an adhesive layer cannot be ensured, but the contact area with respect to a to-be-adhered body falls, and adhesive force falls.
（Ａ）、（Ｃ）成分を併用しそれぞれ、カルボキシル基、スルホン酸基等の酸性官能基を有する（メタ）アクリル系樹脂の場合には、（Ａ）成分は酸価が３５〜１５０ｍｇＫＯＨ／ｇの（メタ）アクリル系樹脂、（Ｃ）成分は酸価が３〜２０ｍｇＫＯＨ／ｇの（メタ）アクリル系樹脂であることが好ましい。（Ａ）成分の酸価が３５ｍｇＫＯＨ／ｇ未満である場合には（Ｄ）成分に対する親和性が低下する。酸価が１５０ｍｇＫＯＨ／ｇを超える場合には、（Ｂ）成分との反応が進行した結果、得られる粘着体の柔軟性が低下し粘着力が低下する。（Ｃ）成分の酸価が３ｍｇＫＯＨ／ｇ未満である場合には（Ｂ）成分と十分に架橋することができず、凝集力が低下し、所望の粘着力を得ることが困難となり、酸価が２０ｍｇＫＯＨ／ｇを超えた場合には（Ｃ）成分の架橋が進行する結果、（Ａ）成分の架橋が阻害され粘着剤としての凝集力が不足することになる。また、（Ｃ）成分の架橋が進行する結果、得られる粘着剤層の柔軟性が低下し、シート状に成形された粘着剤がもろいものとなり、粘着シートの取扱性が低下する。また、凹凸表面を持つ被着体に追従することができないために粘着シートの貼付時の空気等の噛みこみ量が多くなり求める機能性が低下する要因となる。 In the case of a (meth) acrylic resin having (A) and (C) components and having an acidic functional group such as a carboxyl group or a sulfonic acid group, the (A) component has an acid value of 35 to 150 mgKOH / g. The (meth) acrylic resin (C) is preferably a (meth) acrylic resin having an acid value of 3 to 20 mgKOH / g. When the acid value of the component (A) is less than 35 mgKOH / g, the affinity for the component (D) decreases. When an acid value exceeds 150 mgKOH / g, as a result of reaction with (B) component, the softness | flexibility of the adhesive body obtained falls and adhesive force falls. When the acid value of the component (C) is less than 3 mgKOH / g, it cannot be sufficiently crosslinked with the component (B), the cohesive force is lowered, and it becomes difficult to obtain a desired adhesive strength, and the acid value When the amount exceeds 20 mgKOH / g, the crosslinking of the component (C) proceeds. As a result, the crosslinking of the component (A) is inhibited and the cohesive force as an adhesive is insufficient. Moreover, as a result of the progress of the crosslinking of the component (C), the flexibility of the obtained pressure-sensitive adhesive layer is lowered, the pressure-sensitive adhesive formed into a sheet shape becomes brittle, and the handleability of the pressure-sensitive adhesive sheet is lowered. Moreover, since it cannot follow the adherend having an uneven surface, the amount of biting of air or the like when the pressure-sensitive adhesive sheet is stuck increases, resulting in a decrease in required functionality.
（Ａ）成分として、水酸基、アミノ基、アミド基等の塩基性官能基を有する（メタ）アクリル系樹脂の場合に水酸基価は、１０ｍｇＫＯＨ／ｇ以上であることが好ましい。水酸基価が１０ｍｇＫＯＨ／ｇ未満である場合には（Ｂ）成分と十分に反応することができず凝集力が低下し被着体に対する粘着力が低下するからである。 In the case of a (meth) acrylic resin having a basic functional group such as a hydroxyl group, an amino group or an amide group as the component (A), the hydroxyl value is preferably 10 mgKOH / g or more. This is because when the hydroxyl value is less than 10 mgKOH / g, it cannot sufficiently react with the component (B), and the cohesive force is lowered and the adhesive force to the adherend is lowered.
（Ａ）、（Ｃ）成分を併用しそれぞれが、水酸基、アミノ基、アミド基等の塩基性官能基を有する（メタ）アクリル系樹脂の場合には、（Ａ）成分は水酸基価が３５〜１５０ｍｇＫＯＨ／ｇの（メタ）アクリル系樹脂、（Ｃ）成分は水酸基価が３〜２０ｍｇＫＯＨ／ｇの（メタ）アクリル系樹脂であることが好ましい。（Ａ）成分の水酸基価が３５ｍｇＫＯＨ／ｇ未満である場合には（Ｃ）成分に対する親和性が低下する。水酸基価が１５０ｍｇＫＯＨ／ｇを超える場合には、（Ｂ）成分との反応が進行し、得られる粘着シートの柔軟性が低下し粘着力が低下する。（Ｃ）成分の水酸基価が３ｍｇＫＯＨ／ｇ未満である場合には（Ｂ）成分と十分に架橋することができず、凝集力が低下し、所望の粘着力を得ることができず、水酸基価が２０ｍｇＫＯＨ／ｇを超えた場合には（Ｃ）成分の架橋が進行する結果、（Ａ）成分の架橋が阻害され粘着剤としての凝集力が不足することになる。また、（Ｃ）成分の架橋が進行する結果、得られる粘着剤層の柔軟性が低下し、被着体に対する粘着力が低下するからである。 In the case of a (meth) acrylic resin in which the components (A) and (C) are used in combination and each has a basic functional group such as a hydroxyl group, amino group, or amide group, the component (A) has a hydroxyl value of 35 to 35. The 150 mg KOH / g (meth) acrylic resin and the component (C) are preferably (meth) acrylic resins having a hydroxyl value of 3 to 20 mg KOH / g. When the hydroxyl value of the component (A) is less than 35 mgKOH / g, the affinity for the component (C) decreases. When a hydroxyl value exceeds 150 mgKOH / g, reaction with (B) component advances, the softness | flexibility of the adhesive sheet obtained falls and adhesive force falls. When the hydroxyl value of the component (C) is less than 3 mgKOH / g, it cannot be sufficiently crosslinked with the component (B), the cohesive force decreases, the desired adhesive strength cannot be obtained, and the hydroxyl value When the amount exceeds 20 mgKOH / g, the crosslinking of the component (C) proceeds. As a result, the crosslinking of the component (A) is inhibited and the cohesive force as an adhesive is insufficient. Moreover, it is because the softness | flexibility of the adhesive layer obtained as a result of progress of bridge | crosslinking of (C) component falls, and the adhesive force with respect to a to-be-adhered body falls.
本発明において、粘着付与樹脂を併用することができ、テルペン系樹脂、キシレン系樹脂、フェノール樹脂等が挙げられる。この成分を使用することで、粘着力を所望の範囲に調整することが容易になるとともに、粘着剤としての凝集力を高めることもできる。 In the present invention, a tackifier resin can be used in combination, and examples thereof include a terpene resin, a xylene resin, and a phenol resin. By using this component, it becomes easy to adjust the adhesive force to a desired range, and the cohesive force as an adhesive can be increased.
粘着付与樹脂の配合量は、（Ａ）成分１００質量部又は（Ｃ）成分を併用している場合には（Ａ）成分と（Ｃ）成分の合計添加量１００質量部に対して、５〜１５０質量部の範囲内で配合することが好ましい。配合量が５質量部未満であると粘着力向上の効果が表れないため好ましくなく、配合量が１５０質量部より多い場合には粘着剤の靱性が低下するためである。粘着力向上と靱性低下防止の観点から１０〜５０質量部の範囲であることが好ましい。 The compounding amount of the tackifying resin is 5 to 100 parts by mass with respect to 100 parts by mass of the total addition amount of the (A) component and the (C) component when the (A) component 100 parts by mass or the (C) component is used in combination. It is preferable to mix within the range of 150 parts by mass. If the blending amount is less than 5 parts by mass, the effect of improving the adhesive strength is not exhibited, which is not preferable. If the blending amount is more than 150 parts by mass, the toughness of the adhesive decreases. The range of 10 to 50 parts by mass is preferable from the viewpoints of improving adhesive strength and preventing toughness reduction.
［Ｄ成分］
本発明で使用される（Ｄ）成分としては、特に制限されず、従来公知のものを適宜選択して使用することができる。例えば、熱伝導剤、難燃剤、発泡剤、導電剤、磁性剤、抗菌剤等が挙げられる。尚、（Ｄ）成分は単独で用いてもよいし、２種以上を組み合わせて用いてもよい。
[D component]
The component (D) used in the present invention is not particularly limited, and conventionally known components can be appropriately selected and used. For example, a heat conductive agent, a flame retardant, a foaming agent, a conductive agent, a magnetic agent, an antibacterial agent, and the like can be given. In addition, (D) component may be used independently and may be used in combination of 2 or more type.
熱伝導剤としてはアルミナ、酸化マグネシウム、窒化アルミニウム、酸化亜鉛、窒化棚素、窒化珪素、マイカ、シリカ、水酸化マグネシウム、水酸化アルミニウム、銀、銅、アルミニウム、炭化珪素、ダイヤモンド粉末、グラファイト、炭素繊維等が挙げられる。これらの成分は単独で用いてもよいし、２種以上を組み合わせて用いてもよい。 As thermal conductive agents, alumina, magnesium oxide, aluminum nitride, zinc oxide, silicon nitride, silicon nitride, mica, silica, magnesium hydroxide, aluminum hydroxide, silver, copper, aluminum, silicon carbide, diamond powder, graphite, carbon Examples thereof include fibers. These components may be used independently and may be used in combination of 2 or more type.
難燃剤としては有機リン酸エステル系難燃剤、ハロゲン化リン酸エステル系難燃剤、無機リン系難燃剤、ハロゲン化ビスフェノール系難燃剤、ハロゲン化合物系難燃剤、アンチモン系難燃剤、窒素系難燃剤、ほう素系難燃剤、金属塩系難燃剤、無機系難燃剤、珪素系難燃剤等が挙げられる。これらの成分は単独で用いてもよいし、２種以上を組み合わせて用いてもよい。 As flame retardants, organic phosphate ester flame retardant, halogenated phosphate ester flame retardant, inorganic phosphorus flame retardant, halogenated bisphenol flame retardant, halogen compound flame retardant, antimony flame retardant, nitrogen flame retardant, Examples thereof include boron flame retardants, metal salt flame retardants, inorganic flame retardants, and silicon flame retardants. These components may be used independently and may be used in combination of 2 or more type.
発泡剤としては、炭酸アンモニウム、炭酸水素アンモニウム、炭酸水素ナトリウム、亜硝酸アンモニウム、水素化ホウ素ナトリウム、アジド類等の無機系発泡剤；トリクロロモノフルオロメタンやジクロロモノフルオロメタンの如き塩フッ化アルカン、アゾビスイソブチロニトリルやアゾジカルボンアミド、バリウムアゾジカルボキシレートの如きアゾ系化合物、パラトルエンスルホニルヒドラジドやジフェニルスルホン−３，３’−ジスルホニルヒドラジド、４，４’−オキシビス（ベンゼンスルホニルヒドラジド）、アリルビス（スルホニルヒドラジド）の如きヒドラジン系化合物、ｐ−トルイレンスルホニルセミカルバジドや４，４’−オキシビス（ベンゼンスルホニルセミカルバジド）の如きセミカルバジド系化合物、５−モルホリル−１，２，３，４−チアトリアゾールの如きトリアゾール系化合物、Ｎ，Ｎ’−ジニトロソペンタメチレンテトラミンやＮ，Ｎ’−ジメチル−Ｎ，Ｎ’−ジニトロソテレフタルアミドの如きＮ−ニトロソ系化合物等の有機系発泡剤等が挙げられる。これらの成分は単独で用いてもよいし、２種以上を組み合わせて用いてもよい。 Examples of blowing agents include inorganic blowing agents such as ammonium carbonate, ammonium hydrogen carbonate, sodium hydrogen carbonate, ammonium nitrite, sodium borohydride, and azides; fluorinated alkanes such as trichloromonofluoromethane and dichloromonofluoromethane, azo Azo compounds such as bisisobutyronitrile, azodicarbonamide, barium azodicarboxylate, paratoluenesulfonyl hydrazide, diphenylsulfone-3,3′-disulfonylhydrazide, 4,4′-oxybis (benzenesulfonylhydrazide), Hydrazine compounds such as allyl bis (sulfonylhydrazide), semicarbazide compounds such as p-toluylenesulfonyl semicarbazide and 4,4′-oxybis (benzenesulfonyl semicarbazide), 5-morpholine -Triazole compounds such as 1,2,3,4-thiatriazole, N-nitroso compounds such as N, N'-dinitrosopentamethylenetetramine and N, N'-dimethyl-N, N'-dinitrosotephthalamide Examples thereof include organic foaming agents such as compounds. These components may be used independently and may be used in combination of 2 or more type.
導電剤としては、例えば、銀、銀合金、金、銅、銅合金、ニッケル、ニッケル合金、錫、錫合金などの導電性金属、酸化インジウム、五酸化アンチモン、アルミン酸亜鉛、アンチモン酸亜鉛等の導電性無機酸化物、アルミナ、ガラスなどの無機絶縁体や、ポリエチレン、ポリスチレンなどの有機高分子化合物などの表面を導電性物質でコートしたもの、ポリアニリンやポリピロール、ポリチオフェン等の導電性高分子、さらにカーボン、グラファイト等の他に、カーボンナノチューブ、カーボンマイクロコイル等が挙げられる。これらの成分は単独で用いてもよいし、２種以上を組み合わせて用いてもよい。 Examples of the conductive agent include conductive metals such as silver, silver alloy, gold, copper, copper alloy, nickel, nickel alloy, tin, and tin alloy, indium oxide, antimony pentoxide, zinc aluminate, and zinc antimonate. Conductive polymers such as inorganic insulators such as conductive inorganic oxides, alumina, and glass, and organic polymer compounds such as polyethylene and polystyrene coated with conductive materials, conductive polymers such as polyaniline, polypyrrole, and polythiophene, In addition to carbon, graphite, etc., carbon nanotubes, carbon microcoils, etc. can be mentioned. These components may be used independently and may be used in combination of 2 or more type.
磁性剤としては、例えば、ヘマタイト、鉄粉、マグネタイト、フェライト等が挙げられる。これらの成分は単独で用いてもよいし、２種以上を組み合わせて用いてもよい。 Examples of the magnetic agent include hematite, iron powder, magnetite, and ferrite. These components may be used independently and may be used in combination of 2 or more type.
抗菌剤としては、銀、亜鉛、銅、チタン、モリブデン等の金属；これらの金属イオンをシリカ、ゼオライト、合成ゼオライト、リン酸ジルコニウム、リン酸カルシウム、リン酸亜鉛カルシウム、セラミック、アルミナシリコン、チタンゼオライト、アパタイト、炭酸カルシウム等の無機質微粒子に担持させたもの；ゾルーゲル法により無機化合物粒子の表面を他の無機酸化物、複合酸化物等により積層又は被覆等したもの等の無機系抗菌剤、イソチオシアン酸アリル、ポリオキシアルキレントリアルキルアンモニウム、塩化べンザルコニウム、へキサメチレンビグアニド塩酸塩、有機シリコーン第４級アンモニウム塩、塩化ベンザルコニウム等の第４級アンモニウム塩類、フェニルアミド系化合物、ビグアニド系化合物、スルホイソフタル酸テトラアルキルホスホニウム塩、安息香酸、安息香酸塩類、サリチル酸、サリチル酸塩類、フェノール、ソルビン酸及びその塩類、デヒドロ酢酸及びその塩類、パラオキシ安息香酸エステル（パラベン）、ポリリジン又はポリリジン塩、アンモニウム塩基、ホスホニウム塩基、スルホニウム塩基、フェニルアミド基、ビグアニド基等の抗菌活性基を主鎖又は側鎖に有する高分子化合物等の有機系抗菌剤が挙げられる。これらの成分は単独で用いてもよいし、２種以上を組み合わせて用いてもよい。 Antibacterial agents include metals such as silver, zinc, copper, titanium, and molybdenum; these metal ions are silica, zeolite, synthetic zeolite, zirconium phosphate, calcium phosphate, zinc calcium phosphate, ceramic, alumina silicon, titanium zeolite, and apatite. Supported on inorganic fine particles such as calcium carbonate; inorganic antibacterial agents such as those obtained by laminating or coating the surface of inorganic compound particles with other inorganic oxides, composite oxides, etc. by sol-gel method, allyl isothiocyanate, Polyoxyalkylene trialkyl ammonium, benzalkonium chloride, hexamethylene biguanide hydrochloride, quaternary ammonium salts such as organic silicone quaternary ammonium salt, benzalkonium chloride, phenylamide compound, biguanide compound, sulfoisophthalic acid Traalkylphosphonium salts, benzoic acid, benzoates, salicylic acid, salicylates, phenol, sorbic acid and salts thereof, dehydroacetic acid and salts thereof, paraoxybenzoic acid ester (paraben), polylysine or polylysine salt, ammonium base, phosphonium base, Examples thereof include organic antibacterial agents such as a polymer compound having an antibacterial active group such as a sulfonium base, a phenylamide group or a biguanide group in the main chain or side chain. These components may be used independently and may be used in combination of 2 or more type.
（Ｄ）成分の配合割合はその使用目的に応じて適宜選択することができる。（Ｄ）成分の粘着剤中の配合割合が５０体積％〜８０体積％であることが必要である。５０体積％未満である場合には、目的とする機能を発現することが困難となるし、８０体積％を超える場合には、粘着剤の粘度が上昇し、シート状に成形することが困難となるからである。 (D) The mixture ratio of a component can be suitably selected according to the use purpose. (D) It is necessary for the mixture ratio in the adhesive of a component to be 50 volume%-80 volume%. If it is less than 50% by volume, it will be difficult to develop the intended function, and if it exceeds 80% by volume, the viscosity of the adhesive will increase, making it difficult to form a sheet. Because it becomes.
（Ｄ）成分の形状は、球状又は擬球状であることが好ましい。平板状、針状などアスペクト比の高いものは、粘着剤層の厚み方向の柔軟性が低下し、被着体に対する粘着力を低下させる要因となるからである。 The shape of component (D) is preferably spherical or pseudospherical. This is because those having a high aspect ratio such as a flat plate shape or a needle shape decrease the flexibility in the thickness direction of the pressure-sensitive adhesive layer, and cause a decrease in the adhesive force to the adherend.
また、（Ｄ）成分が球状又は擬球状である場合、その平均粒子径は０．０１〜５０μｍ程度であることが好ましい。平均粒子径が０．０１μｍ未満では粒子の自己凝集性の制御が困難であること、フィラーが高価でありコストが増大することとなるからである。平均粒子径が５μｍを超えると前記（Ａ）成分中に充填させることが困難となるからである。自己凝集性の制御と充填性の観点から０．０２〜２０μｍの範囲であることが好ましい。
尚、粘着剤層の平滑性を確保することが困難となるため、（Ｄ）成分が球状又は揮球状である場合、その最大粒子径が粘着剤層の厚みより小さい粒子径のものを使用することが好ましい。
In addition, when the component (D) is spherical or pseudospherical, the average particle size is preferably about 0.01 to 50 μm. This is because if the average particle size is less than 0.01 μm, it is difficult to control the self-aggregation property of the particles, and the filler is expensive and the cost is increased. It is because it becomes difficult to fill the component (A) when the average particle diameter exceeds 5 μm. The range of 0.02 to 20 μm is preferable from the viewpoint of self-aggregation control and filling properties.
In addition, since it becomes difficult to ensure the smoothness of the pressure-sensitive adhesive layer, when the component (D) is spherical or volatile, the one having a maximum particle size smaller than the thickness of the pressure-sensitive adhesive layer is used. It is preferable.
さらに、（Ｄ）成分が球状又は擬球状である場合、平均粒子径の異なるものを組み合わせて用いることが好ましい。このようにして平均粒子径の異なるものを数種類組み合わせ、粘着剤中に混在させることによって、得られる粘着剤の粘度を低下させることが可能となり、同じ平均粒子径のものを組み合わせるより高充填することが可能となる。具体的には、（Ｄ１）平均粒子径が１０〜５０μｍ、（Ｄ２）平均粒子径０．０１〜５μｍのものを７０：３０〜５０：５０の範囲で組み合わせることが好ましい。（Ｄ１）成分が上記範囲より多い場合には、粘着剤層の平滑性を維持することが困難となり、上記範囲より少ない場合には、（Ｄ）成分同士の接触頻度が低下し、機能性が低下するためである。尚、（Ｄ１）、（Ｄ２）成分とも先に（Ｄ）成分で挙げたものを使用することができ、上記平均粒子径を満足する限りにおいては、２種以上のものを組み合わせて用いてもよい。 Furthermore, when the component (D) is spherical or pseudospherical, it is preferable to use a combination of those having different average particle diameters. By combining several types with different average particle diameters in this way and mixing them in the pressure-sensitive adhesive, it becomes possible to reduce the viscosity of the resulting pressure-sensitive adhesive, and filling higher than combining those with the same average particle diameter Is possible. Specifically, it is preferable to combine those having (D1) an average particle diameter of 10 to 50 μm and (D2) an average particle diameter of 0.01 to 5 μm in the range of 70:30 to 50:50. When the component (D1) is more than the above range, it becomes difficult to maintain the smoothness of the pressure-sensitive adhesive layer. When the component is less than the above range, the contact frequency between the components (D) decreases, and the functionality is improved. It is because it falls. In addition, as the components (D1) and (D2), those mentioned above as the component (D) can be used. As long as the average particle diameter is satisfied, two or more types may be used in combination. Good.
［粘着シート］
本発明の粘着シートは、本発明の粘着剤そのものをフイルム状ないしシート状に形成するか、フイルム状ないしシート状の基材の片面若しくは両面に本発明の粘着剤を設けることにより実現することができる。
[Adhesive sheet]
The pressure-sensitive adhesive sheet of the present invention can be realized by forming the pressure-sensitive adhesive of the present invention itself in a film or sheet form, or by providing the pressure-sensitive adhesive of the present invention on one or both sides of a film or sheet-like substrate. it can.
本発明の粘着シートは、その構成要素として、基材及び／又は粘着剤層を備える。以下、各要素について説明する。 The pressure-sensitive adhesive sheet of the present invention includes a substrate and / or a pressure-sensitive adhesive layer as its constituent elements. Hereinafter, each element will be described.
［基材］
本発明にいう「基材」とは、粘着剤層を支持するための部材であって、フイルム状ないしシート状を呈するものである。本明細書において「フイルム状ないしシート状」というときは、薄膜状ないし薄板状の形状を意味し、通常は４〜２５０μｍの厚さのものが用いられる。
[Base material]
The “base material” referred to in the present invention is a member for supporting the pressure-sensitive adhesive layer and exhibits a film shape or a sheet shape. In the present specification, the term “film shape or sheet shape” means a thin film shape or a thin plate shape, and usually has a thickness of 4 to 250 μm.
基材の構成材料については特に限定されず、従来、粘着シート用の基材として用いられてきた材料の中から、粘着シートの用途に応じて適宜選択することができる。具体的には、ポリエチレンテレフタレート、ポリエチレンナフタレート、ポリプチレンテレフタレート、ポリエチレン、ポリプロピレン、ポリカーボネート、トリアセチルセルロース、セロハン、ポリイミド、ポリアミド、ポリフェニレンスルフイド、ポリエーテルイミド、ポリエーテルスルホン、芳香族ポリアミド、若しくはポリスルホン等の合成樹脂、金属等の中から選択することができる。尚、基材は透明であっても、着色せしめたものであってもよい。着色は、基材の構成材料に各種顔料や染料を配合する方法等により行うことができる。また、基材の表面は平滑であるものに限定されず、その表面がマット状に加工されているものであってもよい。 The constituent material of the base material is not particularly limited, and can be appropriately selected from materials conventionally used as the base material for pressure-sensitive adhesive sheets according to the use of the pressure-sensitive adhesive sheet. Specifically, polyethylene terephthalate, polyethylene naphthalate, polyethylene terephthalate, polyethylene, polypropylene, polycarbonate, triacetyl cellulose, cellophane, polyimide, polyamide, polyphenylene sulfide, polyether imide, polyether sulfone, aromatic polyamide, or It can be selected from synthetic resins such as polysulfone and metals. The base material may be transparent or colored. Coloring can be performed by a method of blending various pigments or dyes into the constituent material of the substrate. The surface of the substrate is not limited to a smooth surface, and the surface may be processed into a mat shape.
基材は、その構成材料中に、従来公知の添加剤、具体的には、耐熱安定剤、耐酸化安定剤、耐侯安定剤、紫外線吸収剤、帯電防止剤等を含有するものであってもよい。また、粘着層との密着性を向上させることを目的として、表面処理を施したものを用いることが好ましい。表面処理としては、例えばコロナ放電処理・グロー放電処理等の放電処理、プラズマ処理、火炎処理、オゾン処理、紫外線処理・電子線処理・放射線処理等の電離活性線処理、サンドマット処理・アンカー処理・へアライン処理・エンボス加工等の粗面化処理、化学薬品処理、易接着層塗布処理等が挙げられる。 The base material may contain a conventionally known additive, specifically, a heat resistance stabilizer, an oxidation resistance stabilizer, an anti-glare stabilizer, an ultraviolet absorber, an antistatic agent, etc. in its constituent materials. Good. Moreover, it is preferable to use what gave surface treatment for the purpose of improving adhesiveness with an adhesion layer. Examples of the surface treatment include discharge treatment such as corona discharge treatment and glow discharge treatment, plasma treatment, flame treatment, ozone treatment, ionizing active ray treatment such as ultraviolet treatment, electron beam treatment and radiation treatment, sand mat treatment and anchor treatment, Examples thereof include roughening treatment such as hair alignment treatment and embossing treatment, chemical treatment, and easy adhesion layer coating treatment.
［粘着剤層］
本発明にいう「粘着剤層」とは、基材の少なくとも一方の表面を被覆するように形成された層であり、（Ａ）活性水素含有基を有する（メタ）アクリル系樹脂及び（Ｂ）所定の官能基当量を有するアクリル系架橋剤を含有する粘着剤からなるものである。
[Adhesive layer]
The “pressure-sensitive adhesive layer” referred to in the present invention is a layer formed so as to cover at least one surface of a substrate, and (A) a (meth) acrylic resin having an active hydrogen-containing group and (B) It consists of an adhesive containing an acrylic crosslinking agent having a predetermined functional group equivalent.
粘着剤層の厚さはその使用目的に応じ適宜選択されるものであるが、一般に１０〜１５０μｍとすることが好ましい。１０μｍ未満の場合には、被着体に対する充分な粘着力が得られなくなるため好ましくなく、１５０μｍを超える場合には乾燥不良を起こすおそれがある点において好ましくない。被着体に対する粘着力と乾燥不良を防止する点から２０〜８０μｍとすることが更に好ましく、３０〜６０μｍとすることが特に好ましい。 Although the thickness of an adhesive layer is suitably selected according to the intended purpose, generally it is preferable to set it as 10-150 micrometers. When the thickness is less than 10 μm, it is not preferable because sufficient adhesion to the adherend cannot be obtained, and when it exceeds 150 μm, it is not preferable in that a drying failure may occur. From the point which prevents the adhesive force with respect to a to-be-adhered body, and drying defect, it is still more preferable to set it as 20-80 micrometers, and it is especially preferable to set it as 30-60 micrometers.
［粘着シート］
本発明の粘着シートは、前記（Ａ）成分、（Ｂ）成分及び（Ｄ）成分、所望により（Ｃ）成分等のその他の成分を適当な溶剤に溶解し、或いは分散させて、固形分濃度を３０〜９０質量％程度の粘着剤層形成塗工液とし、この粘着剤層形成塗工液を常法に従って、基材の片面若しくは両面の表面を被覆するように塗布し、これを乾燥する方法により得ることができる。尚、基材に代えて離型性を有するフイルムを用い、離型性を有する表面に粘着剤層形成塗工液を塗布・乾燥させフイルム状ないしシート状に形成して粘着剤層のみからなる粘着シートとすることができる。
[Adhesive sheet]
The pressure-sensitive adhesive sheet of the present invention is obtained by dissolving or dispersing the above components (A), (B) and (D), and other components such as component (C) , if necessary, in an appropriate solvent. Is applied to form a pressure-sensitive adhesive layer-forming coating solution of about 30 to 90% by mass, and this pressure-sensitive adhesive layer-forming coating solution is applied so as to cover one or both surfaces of the substrate according to a conventional method and dried. It can be obtained by a method. In addition, it uses a film having releasability in place of the base material, and a pressure-sensitive adhesive layer forming coating solution is applied to the surface having releasability and dried to form a film or sheet, and consists only of the pressure-sensitive adhesive layer. It can be set as an adhesive sheet.
この際、粘着剤層形成塗工液には、従来慣用されている各種添加剤、例えば、重合反応禁止剤、架橋促進剤、酸化防止剤、安定剤、カップリング剤等を添加してもよい。 At this time, various conventionally used additives such as a polymerization reaction inhibitor, a crosslinking accelerator, an antioxidant, a stabilizer, a coupling agent and the like may be added to the pressure-sensitive adhesive layer forming coating solution. .
前記架橋促進剤としては、例えば、トリエチルアミン系、ナフテン酸コバルト系、スズ系の架橋促進剤が挙げられ、特に、塩化第−スズ、テトラーｎ−ブチルスズ、水酸化トリメチルスズ、塩化ジメチルスズ、ジラタリン酸ジーｎ−ブチルスズ等のスズ系架橋促進剤を使用することが好ましい。架橋促進剤を使用することでより低温・短時間で架橋することが可能となる。この他、酸化防止剤としては、フェノール系酸化防止剤等が挙げられる。 Examples of the crosslinking accelerator include triethylamine-based, cobalt naphthenate-based, and tin-based crosslinking accelerators, and in particular, stannic chloride, tetra-n-butyltin, trimethyltin hydroxide, dimethyltin chloride, dilatate phosphate It is preferable to use a tin-based crosslinking accelerator such as n-butyltin. By using a crosslinking accelerator, crosslinking can be performed at a lower temperature and in a shorter time. In addition, examples of the antioxidant include phenolic antioxidants.
塗布の方法については特に制限はなく、ワイヤーバー、アプリケー夕―、刷毛、スプレー、ローラー、グラビアコー夕ー、ダイコーター、リップコー夕ー、コンマコー夕ー、ナイフコー夕―、リバースコー夕ー、スピンコー夕ー等を用いた従来公知の塗布方法を利用することができる。尚、粘着剤層形成塗工液を塗布する基材や離型性を有するフイルムの面には、必要に応じて予め表面処理を施しておいてもよい。 There are no particular restrictions on the method of application: wire bar, application evening, brush, spray, roller, gravure coating, die coater, lip coating, comma coating, knife coating, reverse coating, spin coating. A conventionally known coating method using a coating etc. can be used. In addition, you may surface-treat in advance as needed to the surface of the base material which apply | coats an adhesive layer formation coating liquid, or the film which has mold release property.
乾燥方法についても特に制限はなく、熱風乾燥、減圧乾燥等の従来公知の乾燥方法を利用することができる。乾燥条件については、粘着剤の種類や塗工液で使用した溶剤の種類、粘着剤層の膜厚等に応じて適宜設定すればよいが、６０〜２００℃程度の温度で乾燥を行うことが一般的である。 There is no restriction | limiting in particular also about a drying method, Conventionally well-known drying methods, such as hot air drying and reduced pressure drying, can be utilized. About drying conditions, what is necessary is just to set suitably according to the kind of adhesive, the kind of solvent used by coating liquid, the film thickness of an adhesive layer, etc., but drying at the temperature of about 60-200 ° C. It is common.
本発明の粘着シートにおいて、フィラーとして熱伝導剤を使用した場合の熱伝導度は、熱の放散性を十分発現させるため、０．８Ｗ・ｍ−１・Ｋ−１以上であることが好ましい。３．０Ｗ・ｍ−１・Ｋ−１以上であると更に好ましく、５．０Ｗ・ｍ−１・Ｋ−１以上であることが特に好ましい。 In the pressure-sensitive adhesive sheet of the present invention, the thermal conductivity when a thermal conductive agent is used as the filler is preferably 0.8 W · m−1 · K−1 or more in order to sufficiently exhibit heat dissipation. More preferably, it is 3.0 W · m−1 · K−1 or more, and particularly preferably 5.0 W · m−1 · K−1 or more.
本発明の粘着シートにおいて、フィラーとして熱伝導剤を使用した場合の２３℃における１８０°粘着力は、アルミニウムを被着体とした際に１．０Ｎ／２５ｍｍ以上であることが好ましい。被着体に対する密着性を確保し、熱の放散性を十分発現させるためである。粘着力が１．５Ｎ／２５ｍｍ以上であると更に好ましく、３．０Ｎ／２５ｍｍ以上であることが特に好ましい。 In the pressure-sensitive adhesive sheet of the present invention, the 180 ° adhesive strength at 23 ° C. when a heat conductive agent is used as the filler is preferably 1.0 N / 25 mm or more when aluminum is used as the adherend. This is because the adhesion to the adherend is ensured and the heat dissipation property is sufficiently developed. The adhesive strength is more preferably 1.5 N / 25 mm or more, and particularly preferably 3.0 N / 25 mm or more.
本発明の粘着シートにおいて、粘着剤層の引張破断伸びは５．０％以上であることが好ましい。引張破断伸びが５．０％未満であると粘着剤層がもろく、柔軟性を損ない被着体に対する密着性を確保できないからである。３０％以上であることが更に好ましく、１００％以上であることが特に好ましい。 In the pressure-sensitive adhesive sheet of the present invention, the tensile elongation at break of the pressure-sensitive adhesive layer is preferably 5.0% or more. This is because if the tensile elongation at break is less than 5.0%, the pressure-sensitive adhesive layer is fragile and the flexibility is impaired, and adhesion to an adherend cannot be secured. More preferably, it is 30% or more, and particularly preferably 100% or more.
本発明の粘着シートにおいて、フィラーとして難燃剤を使用した場合の難燃性は、着火延焼の危険性を排除する観点からＵＬ９４−ＶＴＭ−０の規格を満足する必要がある。 In the pressure-sensitive adhesive sheet of the present invention, the flame retardancy when a flame retardant is used as a filler needs to satisfy the UL94-VTM-0 standard from the viewpoint of eliminating the risk of ignition and fire spread.
［使用方法］
本発明の粘着シートにおいて、フィラーとして熱伝導剤を使用した場合には、ＩＣパッケージやトランジスタ、ダイオード等の電子部品又はプラズマディスプレイや、液晶ディスプレイのパネル等の発熱体とヒートシンクや放熱金属板等の放熱体との間に介在することにより、放熱体から発生する熱を効率的に外部に放出させる熱伝導粘着シートとして使用することができる。更に、フィラーとして難燃剤を使用した場合には難燃性シートとして、発泡剤を使用した場合には、被着体間に粘着シートを挟み加熱発泡させることにより、隙間充填性シートとして使用することができる。導電剤を使用した場合には導電性シートとして使用することができる。
[how to use]
In the pressure-sensitive adhesive sheet of the present invention, when a heat conductive agent is used as a filler, an electronic component such as an IC package, a transistor, or a diode, or a plasma display, a heating element such as a liquid crystal display panel, a heat sink, a heat dissipation metal plate, etc. By interposing between it and the heat radiating body, it can be used as a heat conductive adhesive sheet that efficiently releases the heat generated from the heat radiating body to the outside. Furthermore, when a flame retardant is used as a filler, as a flame retardant sheet, when a foaming agent is used, it is used as a gap filling sheet by sandwiching an adhesive sheet between adherends and heating and foaming. Can do. When a conductive agent is used, it can be used as a conductive sheet.
以下、本発明の粘着シートにつき実施例を用いて具体的に説明するが、本発明の粘着シートはこれらの実施例によって何ら限定されるものではない。尚、実施例、比較例中の粘着剤については均一性を、粘着シートについては粘着力、柔軟性の各項目を評価した。尚フィラーとして熱伝導剤を使用した場合には熱伝導度の評価を、難燃剤を使用した場合には難燃性の各評価を追加し評価した。尚、これらの項目については、以下の方法により評価した。 Hereinafter, although it demonstrates concretely using an Example about the adhesive sheet of this invention, the adhesive sheet of this invention is not limited at all by these Examples. In addition, uniformity was evaluated about the adhesive in an Example and a comparative example, and each item of adhesive force and a softness | flexibility was evaluated about the adhesive sheet. In addition, when the heat conductive agent was used as a filler, evaluation of heat conductivity was added, and when a flame retardant was used, each evaluation of flame retardance was added and evaluated. These items were evaluated by the following methods.
（均一性）
後述する粘着剤層形成塗工液の状態を目視にて評価した。
評価基準は以下の通りである。
Ｏ：分離・沈殿等が見られない。
×：分離・沈殿等が見られる。
(Uniformity)
The state of the pressure-sensitive adhesive layer forming coating solution described later was visually evaluated.
The evaluation criteria are as follows.
O: Separation / precipitation is not observed.
X: Separation / precipitation is observed.
（粘着力）
粘着剤層形成塗工液を基材厚み１００μｍのＰＥＴフイルム上に粘着剤層の厚みが１００μｍとなるよう塗布・乾燥させ、厚さ１０Ｏμｍの剥離フイルム（シリコーン処理ポリエチレンテレフタレート）と貼着し、４０℃で７日間養生することにより粘着シートを作製した。このシートをＪＩＳ Ｚ０２３７の規定に基づき、試験片幅を２５ｍｍ、被着体をアルミ板（番手：Ａ１０５０）として２３℃における１８０°粘着力を測定した。このものの物性を表１に示す。
(Adhesive force)
The pressure-sensitive adhesive layer-forming coating solution was applied and dried on a PET film having a substrate thickness of 100 μm so that the pressure-sensitive adhesive layer had a thickness of 100 μm, and adhered to a 10 Oμm-thick release film (silicone-treated polyethylene terephthalate). An adhesive sheet was prepared by curing at 7 ° C. for 7 days. Based on JIS Z0237, this sheet was measured for 180 ° adhesive strength at 23 ° C. with a test piece width of 25 mm and an adherend as an aluminum plate (count: A1050). The physical properties of this product are shown in Table 1.
（柔軟性）
ＪＩＳ Ｐ８１１３の規定の基づき、熊谷理機工業社製横型引張強度試験機（卓上型）を用いて測定を行った。粘着剤層形成塗工液を基材厚み１００μｍの剥離フイルム（シリコーン処理ポリエチレンテレフタレート）上に粘着剤層の厚みが１００μｍとなるよう塗布・乾燥させ、厚さ１０Ｏμｍの剥離フイルムと貼着し、４０℃で７日間養生することにより粘着シートを作製した。このシートを、幅１０ｍｍ、長さ４０ｍｍに切断し、剥離フイルムを取り除き試験片とした。この試験片をチャック間距離３０ｍｍ、速度２０ｍｍ／ｍｉｎの条件で水平方向に引っ張り、引張破断伸びを測定した。
(Flexibility)
Based on the provisions of JIS P8113, measurement was performed using a horizontal tensile strength tester (desktop type) manufactured by Kumagai Riki Kogyo Co., Ltd. The pressure-sensitive adhesive layer-forming coating solution was applied and dried on a release film (silicone-treated polyethylene terephthalate) having a substrate thickness of 100 μm so that the thickness of the pressure-sensitive adhesive layer was 100 μm, and adhered to a release film having a thickness of 10 Oμm. An adhesive sheet was prepared by curing at 7 ° C. for 7 days. This sheet was cut into a width of 10 mm and a length of 40 mm, and the release film was removed to obtain a test piece. The test piece was pulled in the horizontal direction under conditions of a distance between chucks of 30 mm and a speed of 20 mm / min, and the tensile elongation at break was measured.
（熱伝導度）
フィラーとして、熱伝導剤を使用し、粘着剤層形成塗工液を基材厚み１００μｍの剥離フイルム（シリコーン処理ポリエチレンテレフタレート）上に粘着剤層の厚みが１００μｍとなるよう塗布・乾燥させ、厚さ１０Ｏμｍの剥離フイルムと貼着し、４０℃で７日間養生することにより熱伝導粘着シートを作製した。このシートを、幅１０ｍｍ、長さ４０ｍｍに切断し、剥離フイルムを取り除き試験片とした。この試験片をＩＳＯ２２００７−３の規定に基づき、株式会社アイフェイズ製アイフェイズモバイル１Ｕにより、熱拡散率を測定した。また、ＪＩＳ Ｋ７１１２に規定に基づき熱伝導性粘着剤の密度を、ＪＩＳ Ｋ７１２３の規定に基づき比熱を測定し、これらのパラメータから熱伝導度を算出した。
(Thermal conductivity)
A heat conductive agent is used as a filler, and the adhesive layer forming coating solution is applied and dried on a peeling film (silicone-treated polyethylene terephthalate) having a substrate thickness of 100 μm so that the thickness of the adhesive layer is 100 μm, and the thickness is increased. A heat conductive pressure-sensitive adhesive sheet was prepared by pasting with a 10 Om release film and curing at 40 ° C for 7 days. This sheet was cut into a width of 10 mm and a length of 40 mm, and the release film was removed to obtain a test piece. The thermal diffusivity of this test piece was measured with Eye Phase Mobile 1U manufactured by Eye Phase Co., Ltd. based on the provisions of ISO 22007-3. Moreover, the density of the heat conductive adhesive was measured based on the specification of JIS K7112, the specific heat was measured based on the specification of JIS K7123, and the thermal conductivity was calculated from these parameters.
（難燃性）
ＵＬ９４難燃性規格に準拠して、実施例の粘着シートの難燃性を評価した。評価基準は以下の通りである。
○：ＵＬ９４ＶＴＭ−０基準を満足する難燃性を示した場合。
×：ＵＬ９４ＶＴＭ−０基準を満足しなかった場合。
(Flame retardance)
Based on UL94 flame retardancy standard, the flame retardance of the adhesive sheet of an Example was evaluated. The evaluation criteria are as follows.
○: When flame retardancy satisfying the UL94VTM-0 standard is shown.
×: When the UL94VTM-0 standard was not satisfied.
各実施例、比較例で用いた各成分は以下のとおりである。 Each component used in each example and comparative example is as follows.
（Ａ１成分）
質量平均分子量３０００、酸価９８ｍｇＫＯＨ／ｇ、ガラス転移温度−３０℃のアクリル系樹脂である。構成モノマーとして、アクリル酸ブチル、アクリル酸を含むものである。
(A1 component)
It is an acrylic resin having a mass average molecular weight of 3000, an acid value of 98 mgKOH / g, and a glass transition temperature of −30 ° C. Constituent monomers include butyl acrylate and acrylic acid.
（Ａ２成分）
質量平均分子量３０００、酸価６０ｍｇＫＯＨ／ｇ、ガラス転移温度−５４℃のアクリル系樹脂である。構成モノマーとして、アクリル酸２−エチルヘキシル、アクリル酸を含むものである。
(A2 component)
It is an acrylic resin having a mass average molecular weight of 3000, an acid value of 60 mgKOH / g, and a glass transition temperature of −54 ° C. As a constituent monomer, 2-ethylhexyl acrylate and acrylic acid are included.
（Ａ３成分）
質量平均分子量３０００、酸価９８ｍｇＫＯＨ／ｇ、ガラス転移温度−５４℃のアクリル系樹脂である。構成モノマーとして、アクリル酸２−エチルヘキシル、アクリル酸を含むものである。
(A3 component)
It is an acrylic resin having a mass average molecular weight of 3000, an acid value of 98 mgKOH / g, and a glass transition temperature of −54 ° C. As a constituent monomer, 2-ethylhexyl acrylate and acrylic acid are included.
（Ａ４成分）
質量平均分子量２０００、水酸基価１１０ｍｇＫＯＨ／ｇ、ガラス転移温度−６０℃のアクリル系樹脂である。構成モノマーとして、アクリル酸２−エチルヘキシル、メタクリル酸２−ヒドロキシエチルを含むものである。
(A4 component)
It is an acrylic resin having a mass average molecular weight of 2000, a hydroxyl value of 110 mgKOH / g, and a glass transition temperature of −60 ° C. Constituent monomers include 2-ethylhexyl acrylate and 2-hydroxyethyl methacrylate.
（Ｂ１）成分
エポキシ基含有アクリル樹脂（エポキシ当量７１０ｇ／ｅｑ、分子量２９００、ガラス転移温度―５７℃）である。
(B1) Component Epoxy group-containing acrylic resin (epoxy equivalent 710 g / eq, molecular weight 2900, glass transition temperature -57 ° C.).
（Ｂ２）成分
エポキシ基含有アクリル樹脂（エポキシ当量１４３０ｇ／ｅｑ、分子量３０００、ガラス転移温度―６１℃）である。
(B2) Component Epoxy group-containing acrylic resin (epoxy equivalent 1430 g / eq, molecular weight 3000, glass transition temperature -61 ° C.).
（Ｂ３）成分
エポキシ基含有アクリル樹脂（エポキシ当量４８０ｇ／ｅｑ、分子量１１０００、ガラス転移温度６３℃）である。
(B3) Component Epoxy group-containing acrylic resin (epoxy equivalent 480 g / eq, molecular weight 11000, glass transition temperature 63 ° C.).
（Ｂ４）成分
イソシアネート基含有アクリル樹脂（イソシアネート当量８５０ｇ／ｅｑ、分子量４，５００、ガラス転移温度−５７℃）である。
(B4) Component isocyanate group-containing acrylic resin (isocyanate equivalent 850 g / eq, molecular weight 4,500, glass transition temperature −57 ° C.).
（Ｃ１成分）
質量平均分子量１３０万、酸価８ｍｇＫＯＨ／ｇ、ガラス転移温度−４０℃のアクリル系樹脂である。構成モノマーとして、アクリル酸ブチル、アクリル酸を含むものである。
(C1 component)
It is an acrylic resin having a mass average molecular weight of 1.3 million, an acid value of 8 mgKOH / g, and a glass transition temperature of −40 ° C. Constituent monomers include butyl acrylate and acrylic acid.
（Ｃ２成分）
質量平均分子量２７万、酸価１５ｍｇＫＯＨ／ｇ、ガラス転移温度−３０℃のアクリル系樹脂である。構成モノマーとして、アクリル酸２−エチルヘキシル、アクリル酸を含むものである。
(C2 component)
It is an acrylic resin having a mass average molecular weight of 270,000, an acid value of 15 mgKOH / g, and a glass transition temperature of -30 ° C. As a constituent monomer, 2-ethylhexyl acrylate and acrylic acid are included.
（Ｃ３成分）
質量平均分子量８１万、酸価２３ｍｇＫＯＨ／ｇ、ガラス転移温度−３０℃のアクリル系樹脂である。構成モノマーとして、アクリル酸２−エチルヘキシル、アクリル酸を含むものである。
(C3 component)
It is an acrylic resin having a mass average molecular weight of 810,000, an acid value of 23 mgKOH / g, and a glass transition temperature of −30 ° C. As a constituent monomer, 2-ethylhexyl acrylate and acrylic acid are included.
（Ｃ４成分）
質量平均分子量９０万、水酸基価６．５ｍｇＫＯＨ／ｇ、ガラス転移温度−６０℃のアクリル系樹脂である。構成モノマーとして、アクリル酸２エチルヘキシル、メタクリル酸２−ヒドロキシエチルを含むものである。
(C4 component)
It is an acrylic resin having a mass average molecular weight of 900,000, a hydroxyl value of 6.5 mgKOH / g, and a glass transition temperature of −60 ° C. Constituent monomers include 2-ethylhexyl acrylate and 2-hydroxyethyl methacrylate.
（Ｃ５成分）
質量平均分子量５２万、水酸基価１５ｍｇＫＯＨ／ｇ、ガラス転移温度−６５℃のアクリル系樹脂である。構成モノマーとして、アクリル酸２−エチルヘキシル、メタクリル酸２−ヒドロキシエチルを含むものである。
(C5 component)
It is an acrylic resin having a mass average molecular weight of 520,000, a hydroxyl value of 15 mgKOH / g, and a glass transition temperature of −65 ° C. Constituent monomers include 2-ethylhexyl acrylate and 2-hydroxyethyl methacrylate.
（Ｄ１−１）成分
平均粒子径２０μｍ、球状のアルミナ粒子である。
(D1-1) Component average particle size 20 μm, spherical alumina particles.
（Ｄ１−２）成分
平均粒子径１８μｍ、水酸化アルミニウム（製品名ハイジライトＨ３１、昭和電工社製）である。
(D1-2) Component average particle diameter 18 μm, aluminum hydroxide (product name: Heidilite H31, manufactured by Showa Denko KK).
（Ｄ２−１）成分
平均粒子径２μｍ、球状のアルミナ粒子である。
(D2-1) Component average particle diameter 2 μm, spherical alumina particles.
（Ｄ２−２）成分
平均粒子径０．２μｍ、球状のアルミナ粒子である。
(D2-2) Component average particle diameter 0.2 μm, spherical alumina particles.
（Ｄ２−３）成分
平均粒子径０．２μｍのシリカである。
(D2-3) Silica having a component average particle size of 0.2 μm.
（粘着付与樹脂）
軟化点１５０℃のテルペンフェノール樹脂である。
(Tackifying resin)
It is a terpene phenol resin having a softening point of 150 ° C.
（その他の樹脂成分）
質量平均分子量３０，０００、酸価７４ｍｇＫＯＨ／ｇ、ガラス転移温度６５℃のアクリル系樹脂である。構成モノマーとして、アクリル酸２エチルヘキシル、アクリル酸を含むものである。
(Other resin components)
It is an acrylic resin having a mass average molecular weight of 30,000, an acid value of 74 mgKOH / g, and a glass transition temperature of 65 ° C. Constituent monomers include 2-ethylhexyl acrylate and acrylic acid.
（その他の架橋剤１）
ダイマー酸ジグリシジルエーテル（エポキシ当量４３０ｇ／ｅｑ、官能基数：２）である。
(Other cross-linking agent 1)
Dimer acid diglycidyl ether (epoxy equivalent: 430 g / eq, number of functional groups: 2).
（その他の架橋剤２）
ＴＥＴＲＡＤ−Ｃ（三菱ガス化学社製、エポキシ当量１００、官能基数：４）である。
(Other cross-linking agent 2)
TETRAD-C (Mitsubishi Gas Chemical Co., Ltd., epoxy equivalent 100, number of functional groups: 4).
（その他の架橋剤３）
エポキシ基含有アクリル樹脂（エポキシ当量１５７０ｇ／ｅｑ、分子量３０００、ガラス転移温度―５８℃）である。
(Other cross-linking agent 3)
It is an epoxy group-containing acrylic resin (epoxy equivalent 1570 g / eq, molecular weight 3000, glass transition temperature -58 ° C.).
（その他の架橋剤４）
ポリグリセロールポリグリシジルエーテル（エポキシ当量１８３ｇ／ｅｑ、官能基数：３）である。
(Other cross-linking agent 4)
Polyglycerol polyglycidyl ether (epoxy equivalent 183 g / eq, functional group number: 3).
（その他の架橋剤５）
ペンタエリスリトールポリグリシジルエーテル（エポキシ当量２２９ｇ／ｅｑ、官能基数：４）である。
(Other cross-linking agent 5)
Pentaerythritol polyglycidyl ether (epoxy equivalent 229 g / eq, functional group number: 4).
（その他の架橋剤６）
エポキシ基含有アクリル樹脂（エポキシ当量１５０ｇ／ｅｑ、分子量３０００、ガラス転移温度―５８℃）である。
(Other cross-linking agent 6)
An epoxy group-containing acrylic resin (epoxy equivalent 150 g / eq, molecular weight 3000, glass transition temperature -58 ° C.).
参考例１
（Ａ１）成分６０質量部、（Ｂ３）成分１０質量部からなる粘着剤組成物にメチルエチルケトン１００質量部、トルエン３０質量部を加え、撹拌、混合することにより粘着剤層形成塗工液を調製した。次に、この塗工液を、厚さ１０Ｏμｍの剥離フイルム（シリコーン処理ポリエチレンテレフタレート）の表面に、ベーカー式アプリケー夕−を用いて塗布し、８０℃で１分、次に１００℃で３分乾燥することにより膜厚１００μｍの粘着層を形成した。この粘着層の前記剥離フイルムとは反対側に厚さ１００μｍの別の剥離フイルム（シリコーン処理ポリエチレンテレフタレート）を貼着し、４０℃で７日間養生することにより粘着シートを作製した。このものの物性を表１に示す。
Reference example 1
A pressure-sensitive adhesive layer-forming coating solution was prepared by adding 100 parts by weight of methyl ethyl ketone and 30 parts by weight of toluene to a pressure-sensitive adhesive composition comprising 60 parts by weight of component (A1) and 10 parts by weight of component (B3). . Next, this coating solution is applied to the surface of a 10 O μm-thick release film (silicone-treated polyethylene terephthalate) using a baker-type application and dried at 80 ° C. for 1 minute and then at 100 ° C. for 3 minutes. As a result, an adhesive layer having a thickness of 100 μm was formed. Another adhesive film (silicone-treated polyethylene terephthalate) having a thickness of 100 μm was stuck on the opposite side of the adhesive layer from the release film, and cured at 40 ° C. for 7 days to prepare an adhesive sheet. The physical properties of this product are shown in Table 1.
実施例２〜１３
表１に示す各成分をそれぞれ用い、参考例１と同様にして粘着シートを作製した。これらの粘着シートの物性を表１に示す。
Examples 2-13
A pressure-sensitive adhesive sheet was prepared in the same manner as in Reference Example 1 using each component shown in Table 1. Table 1 shows the physical properties of these pressure-sensitive adhesive sheets.
比較例１〜８
表２に示す各成分をそれぞれ用い、参考例１と同様にして粘着シートを作製した。これらの粘着シートの物性を表２に示す。尚表中「−」は測定もしくは評価できなかったことを示す。
Comparative Examples 1-8
A pressure-sensitive adhesive sheet was prepared in the same manner as in Reference Example 1 using each component shown in Table 2. Table 2 shows the physical properties of these pressure-sensitive adhesive sheets. In the table, “-” indicates that measurement or evaluation could not be performed.
「評価」
表１で示したように、参考例１は粘着力及び柔軟性に富んだ粘着シートであることが理解できる。実施例２においては参考例１にフィラーを添加したものであるが、この場合においても柔軟性に富んでいることが理解できる。実施例３は架橋剤のガラス転移温度が高いので、柔軟性が低下していることが理解できる。実施例５の熱伝導粘着シートは、官能基当量が大きいものであるため凝集力がやや不足しているため、粘着力が低下したものと推測できる。実施例７はフィラーの充填量が低いため熱伝導度が低いことが理解できる。実施例８においては、フィラーの充填量が多いため、柔軟性は維持しているものの粘着力が低下していることが理解できる。実施例１１においては、難燃剤と熱伝導剤を添加したものであるが、この場合においても柔軟性を確保しつつ熱伝導性と難燃性の双方の特性を有していることが理解できる。実施例１３においてアクリル系架橋剤の官能基をイソシアネートのものに変更した場合でも同様の特性を有していることが理解できる。一方、比較例１においては、エポキシ当量は規定の範囲内にはいっているものの相溶性が悪く粘着力等の評価に供することができなかった。また、比較例２、８においては、架橋後に得られた塗膜は柔軟性に劣り、粘着剤層がもろく基材に対する密着性が低いことが理解できる。比較例３はエポキシ当量が大きいため、凝集力が低く粘着力が不足していることが理解できる。比較例４〜７においては粘着力が低下していることが理解できる。
"Evaluation"
As shown in Table 1, it can be understood that Reference Example 1 is an adhesive sheet rich in adhesive strength and flexibility. In Example 2, the filler was added to Reference Example 1, but in this case, it can be understood that it is rich in flexibility. Since Example 3 has a high glass transition temperature of the crosslinking agent, it can be understood that the flexibility is lowered. Since the heat conductive adhesive sheet of Example 5 has a large functional group equivalent, the cohesive force is slightly insufficient, so that it can be assumed that the adhesive force has decreased. In Example 7, it can be understood that the thermal conductivity is low because the filler filling amount is low. In Example 8, since the filling amount of the filler is large, it can be understood that although the flexibility is maintained, the adhesive strength is reduced. In Example 11, a flame retardant and a heat conducting agent were added, but in this case as well, it can be understood that both the thermal conductivity and the flame retardant properties are obtained while ensuring flexibility. . It can be understood that the same characteristics are obtained even when the functional group of the acrylic crosslinking agent is changed to that of isocyanate in Example 13. On the other hand, in Comparative Example 1, although the epoxy equivalent was within the specified range, the compatibility was poor and it was not possible to evaluate the adhesive strength and the like. Moreover, in Comparative Examples 2 and 8, it can be understood that the coating film obtained after crosslinking is inferior in flexibility, the pressure-sensitive adhesive layer is brittle, and the adhesion to the substrate is low. Since Comparative Example 3 has a large epoxy equivalent, it can be understood that the cohesive force is low and the adhesive strength is insufficient. In Comparative Examples 4-7, it can be understood that the adhesive strength is reduced.
本発明の粘着シートにおいてフィラーとして、熱伝導剤を使用した場合には、熱伝導度と柔軟性に優れるとともに、粘着性も有しているため、半導体集積回路（ＩＣ）パッケージ、トランジスタ若しくはダイオード等の電子部品又は、プラズマディスプレイパネル若しくは液晶ディスプレイパネル等のパネル自体から発生した熱をヒートシンクや放熱金属板等の放熱体に効率よく伝達させるために使用することができる。フィラーを充填した状態で柔軟性に富むものであるため、難燃性と熱伝導性といった複合機能を有する粘着シートとしても利用することができる。 When a thermal conductive agent is used as a filler in the pressure-sensitive adhesive sheet of the present invention, it has excellent thermal conductivity and flexibility, and also has adhesiveness, so that it has a semiconductor integrated circuit (IC) package, transistor, diode, etc. It can be used to efficiently transfer the heat generated from the electronic parts or the panel itself such as a plasma display panel or a liquid crystal display panel to a heat radiating body such as a heat sink or a heat radiating metal plate. Since it is rich in flexibility in a state filled with a filler, it can also be used as an adhesive sheet having a composite function such as flame retardancy and thermal conductivity.
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| JP6423603B2 (en) * | 2014-03-21 | 2018-11-14 | ナミックス株式会社 | Insulating film and semiconductor device |
| JP2016033953A (en) * | 2014-07-31 | 2016-03-10 | 日立化成株式会社 | Temporarily fixing resin composition, temporarily fixing resin film and temporarily fixing resin film sheet |
| CN107849386B (en) * | 2015-07-15 | 2020-04-17 | 株式会社村田制作所 | Composition for forming coating film and electronic component |
| WO2020040177A1 (en) | 2018-08-23 | 2020-02-27 | 三洋化成工業株式会社 | Composition, method for producing said composition, urethane resin, and cooling component and article provided with said urethane resin |
| JP7278810B2 (en) * | 2019-03-14 | 2023-05-22 | 株式会社クラレ | Acrylic resin film and its manufacturing method |
| CN115052947A (en) * | 2020-01-28 | 2022-09-13 | 积水化学工业株式会社 | Adhesive tape |
| JP7472755B2 (en) | 2020-10-27 | 2024-04-23 | ａｒｔｉｅｎｃｅ株式会社 | Laminate |
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| JP4709980B2 (en) * | 2005-09-08 | 2011-06-29 | 綜研化学株式会社 | Adhesive layer for EMI film lamination and EMI laminate film |
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